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ANALYTICAL CHEMISTRY LABORATORY MANUAL

EXPERIMENT NO. 8
Determination of Iron by Permanganometry

I. BACKGROUND

A titration which involves reduction and oxidation reaction is called redox titration. An
example of a redox titration is permanganometry. It involves the use of permanganates which are
strong reducing agents. When used as a titrant to oxidize ferrous ion in acidic conditions, the purple
color of the permanganate ion disappears upon contact with the ferrous-containing sample. Below
is the balanced net ionic equation:

MnO4-1 + 5Fe+2 + 8H+ Mn+2 + 5Fe+3 + 4H2O

The titration ends upon the appearance of a faint pink color which persists for 30 seconds. At
the endpoint, all of the ferrous ion have been consumed and converted to ferric ion.

The potassium permanganate solution must be boiled before using to oxidize all of the
contaminants present in the reagent and water. The standard solution must be protected from
light and must be restandardized if solids are detected upon storage.

The potassium permanganate solution can be standardized against a standard sodium oxalate.
Below is the balanced net ionic equation:

5C2O4-2 + 2MnO4-1 + 16H+ 2Mn+2 + 10CO2 + 8H2O

The sodium oxalate solution needs to be heated because it reacts with permanganate
very slowly at room temperature.

II. OBJECTIVES:

At the end of this activity, the students should be able to:

1. understand the concept of redox titration involving permanganate ion
2. calculate the concentration of iron in an unknown sample.

Department of Biochemistry, College of Allied Sciences, De La Salle Medical and Health Sciences Institute, 2022
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ANALYTICAL CHEMISTRY LABORATORY MANUAL

III. MATERIALS

A. The students need to bring the following:

one (1) 250 mL dark colored glass bottle

B. The instructor/technician/custodian should prepare the following:

Reagents
pre-dried standard Na2C2O4 deionized water
FeSO4.7H2O KMnO4
0.90 M H2SO4 2M H3PO4

Instrument
Electric stove

Instrument
None

Others:

C. The students need to borrow the following from the stockroom:

Item Qty. Item Qty.
burette 1 volumetric pipette (25 mL) 1
burette holder 1 erlenmeyer flask (250 mL) 2
deionized water (in wash bottle) 1 thermometer 1
graduated cylinder (100 mL) 1 stirring rod 1
beaker (100 mL) 2

IV. SAFETY

• Wear lab gown and protective goggles at all times.

• Place highly volatile samples under fume hood.
• Wash hands thoroughly with soap and water before leaving the laboratory.

Department of Biochemistry, College of Allied Sciences, De La Salle Medical and Health Sciences Institute, 2022
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ANALYTICAL CHEMISTRY LABORATORY MANUAL

V. PROCEDURE

A. Preparation of KMnO4 Solution

1. Using a 100-mL beaker, weigh 0.64 to 0.65 g KMnO4.
2. Transfer the solids to a 250-mL erlenmeyer flask and add 200 mL deionized
water.
3. Boil the solution gently and keep hot for an hour.
4. Cover and cool.
5. Transfer the solution to a clean colored glass bottle taking care not to include
the solids. Filter using a sintered glass funnel if necessary.

B. Standardization of KMnO4 Solution

1. Using a clean weighing paper, weigh 0.10 to 0.11 g of standard Na2C2O4.
2. Transfer the solids quantitatively to a 250-mL erlenmeyer flask.
3. Add 100 mL of 0.90 M H2SO4 and shake.
4. Heat the solution to 70 - 80 oC.
5. Titrate with the KMnO4 solution while heating until the appearance of a
persistent faint pink color. The temperature should not drop below 60 oC.
6. Record the initial and final volume of KMnO4 solution.
7. Do another trial. If the results of the first and second trial are not close, do a
third trial.
8. For the reagent blank, repeat steps 3 to 5 using another 250-mL erlenmeyer
flask without the addition of Na2C2O4.

C. Determination of Iron in an Unknown Sample

1. Using a volumetric pipette, transfer 25 mL of unknown sample into a 250-
mL erlenmeyer flask.
2. Add 50 mL deionized water and 12 mL of 2 M H3PO4.
3. Titrate the unknown sample with the KMnO4 solution until the appearance of
a persistent faint pink color. Record the initial and final volume of KMnO 4
solution.
4. Do another trial. If the results of the first and second trial are not close, do a
third trial.

WASTE DISPOSAL: Dispose wastes down the sink in running water.

Excess permanganate solution should be disposed in
an inorganic waste container.

Department of Biochemistry, College of Allied Sciences, De La Salle Medical and Health Sciences Institute, 2022
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ANALYTICAL CHEMISTRY LABORATORY MANUAL

DATA REPORT SHEET – EXPERIMENT NO. 8

Determination of Iron by Permanganometry
GROUP NO.:
NAME: CLASS NO.:
SECTION: DATE PERFORMED:
INSTRUCTOR: DATE COMPLETED:

A. Standardization of KMnO4 Solution

Trial 1 Trial 2
Mass of Na2C2O4 (g)

Moles of Na2C2O4 (mol)

Moles of KMnO4 (mol)

Initial volume reading of KMnO4 (mL)

Final volume reading of KMnO4 (mL)

Volume of KMnO4 used (mL)

Blank reading
(Final Volume – Initial Volume; mL)
Adjusted Volume of KMnO4
due to blank (mL)
Molarity of KMnO4

Average molarity of KMnO4

Calculations

Department of Biochemistry, College of Allied Sciences, De La Salle Medical and Health Sciences Institute, 2022
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ANALYTICAL CHEMISTRY LABORATORY MANUAL

B. Determination of Iron in an Unknown Sample

Trial 1 Trial 2
Molarity of KMnO4

Initial volume reading of KMnO4 (mL)

Final volume reading of KMnO4 (mL)

Volume of KMnO4 used (mL)

Moles of KMnO4 (mol)

Moles of Fe (mol)

Mass of Fe (g)

Volume of unknown sample (L)

Concentration of Fe in g/L

Average concentration of Fe in g/L

Calculations

Department of Biochemistry, College of Allied Sciences, De La Salle Medical and Health Sciences Institute, 2022
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ANALYTICAL CHEMISTRY LABORATORY MANUAL

POST-LAB QUESTIONS – EXPERIMENT NO. 8

Determination of Iron by Permanganometry

1. How many moles of Fe2+ react with one mole of MnO4- ?

2. If the iron in pills was Fe3+ instead of Fe2+, could you still use a potassium
permanganate titration to determine the iron concentration? Why?

3. A sample of iron ore weighing 0.7250 g is dissolved in HCl. The ferrous ion in
the solution required 32.76 mL of 0.0420M KMnO 4 to reach the endpoint.
How many moles of Fe+2 were titrated? What was the percentage of iron in
the iron ore?

Department of Biochemistry, College of Allied Sciences, De La Salle Medical and Health Sciences Institute, 2022