Experiment 30

Determination of Iron by Reaction with

Permanganate-A Redox Titration

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otass,i um perman~anate. KMnOj • is widely use~ as an oxidizing agent in volumetric analysis, In acid
P solution, Mn0-1- Ion undergoes reduction to Mn- T as shown rn the following equanon:

•
Since the Mn0-1- ion is violet and the Mn el ion is nearly colorless. the end point in titrations using KMn0-1 as
the titrant can be taken as the first permanent pink color that appears in the solution.
KMn0-1 will be employed in this experiment to determine the percentage of iron in an unknown contain­
ing iront ll ) ammonium sulfate, Fe(NH-1)/S0-1)e ' 6 H 20. The titration. which involves the oxidation of Fee~
ion to Fe'+ by perrnanganate ion. is carried out in sulfuric acid solution to prevent the air oxidation of Fe 2+ .
The end point of the titration is sharpened markedly if phosphoric acid is present. because the Fe'+ ion pro­
duced in the titration forms an essentially colorless complex with the acid.
The number of moles of potassium permanganate used in the titration is equal to the product of the molar­
ity of the KMnO -1 and the volume used, The number of moles of iron present in the sample is obtained from
the balanced equation for the reaction and the amount of MnO-1' ion reacted. The percentage by weight of iron
in the solid sample follows directly.

Experimental Procedure
Obtain from the stockroom a buret and an unknown ironr Ii j sample.
Weigh out accurately on the analytical balance three samples of about 1.0 g of your unknown into clean
250-mL Erlenmeyer tlasks.
Clean your buret thoroughly, Draw about 100 mL of the standard KMnO-1 solution from the carboy in the
laboratory. Rinse the buret with a few milliliters or the KMnO-1 three times. Drain and then fill the buret with
the KMnO -1 solution.
Prepare 150 nil, of I M H 2SO -1 by pouring 25 mL of 6 M H 2SO -1 into 125 mL of H 20, whi le stirring. Add
50 mL of this 1 M H 2SO -1 to one of the iron samples, The sample should dissolve completely. Without delay.
titrate this iron solution with the KMn0-1 solution. When a light-yellow color develops in the iron solution
during the titration. add 3 ml, of 85';( H,P0-1' alliU.I:n Caustic reagent.
Continue the titration until you obtain the first pink color that persists for l5 to 30 seconds. Repeat the
titration with the other two samples.
Optional The KMnO-1 solution can be standardized by the method you used in this experiment.
Fe(NH)clSO)e . 6 HeO is a primary standard with a molar mass equal to 392.2 g. For standardization. use
0.7 ± 0.05 g samples of the primary standard. weighed to (J.OOO I g. Draw 100 mL of the stock KMnO-1 solu­
tion and titrate the samples as you did the unknown,

Optional Experiment: Determine the mass percent of iron in iron supplement tablets if they contain
iron (II). ferrous ion.

DISPOSAL OF REACTION PRODUCTS. Dispose of your titrated solutions as directed by your labo­
ratory supervisor.
... Name Section

Experiment 30

Data and Calculations: Determination of Iron by Reaction with

Permanganate-A Redox Titration

Mass of sample tube plus contents (J

to

Mass after removing Sample I (J

to

Mass after removing Sample II o

to

Mass after removing Sample III o

I::'

Molarity of standard KMn0-l solution M

Sample II III

Initial buret reading mL mL mL

Final buret reading mL mL mL

Volume KMn0-l required mL mL mL

Moles KMn0-l required

Moles Fe 2+ in sample

Mass of Fe in sample g g c
co

Mass of sample o
I::' g 0
b

Percentage of Fe in sample % S!C cle

Unknown no. _ Average 9'c Fe _ %

Standardization of KMn0 4 Optional

Sample IV V VI

Mass of primary standard g ------g ----g

Moles Fe in standard

(continued 011 following page)

244 Experiment 30 Determination of Iron by Reaction with Permanganate-A Redox Titration

Moles KMn0 4 required

Initial buret reading _ _ _ _ _ _ mL _ _ _ _ _ _ mL _ _ _ _ _ _ mL

Final buret reading _ _ _ _ _ _ mL _ _ _ _ _ _ mL _ _ _ _ _ _ mL

Volume KMn0 4 used _ _ _ _ _ _ mL _ _ _ _ _ _ mL _ _ _ _ _ _ mL

Molarity KMn0 4 ______ M ______ M _____ M

Average molarity ______ M

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Name Section

Experiment 30

Advance Study Assignment: Determination of Iron by Reaction with

Permanganate-A Redox Titration

I. Write the balanced net ionic equation for the reaction bel ween MnOj -- ion and Fe c+ ion in acid solution.

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How many moles of Fc c+ ion can be oxidized by 1.2 x 10- 2 moles MnO -1- ion in the reaction in Question I?

moles

3. A solid sample containing some Fe 2+ ion weighs 1.750 g. It requires 36.44 mL 0.0244 M KMn0-l to
titrate the Fe 2+ in the dissolved sample to a pink end point.

a. How many moles Mn0-l- ion are required?

_ _ _ _ _ _ moles

h. How many moles Fe c+ are there in the sample')

_ _ _ _ _ moles

c. How many grams of iron are there in the sample')

d. What is the percent Fe in the sample')

_ _ _ _ _ c!c

4. What is the percent Fe in ironi ll) ammonium sulfate hexahydrate. Fe(NH-IliS0-l)2 . 6 H,O?

. C!
jC