Pharmaceutical Analysis

Laboratory (1216214)

Redox titration of iron supplement

(ferrous sulphate tablet)

Prof. Saleh Abu-Lafi

Faculty of Pharmacy
Al-Quds University

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List of experiments:
•Experiment 1: Preparation of standard solutions, standardization of HCl
•Experiment 2: Determination of Aspirin using back titration
•Experiment 3: Precipitation titration of potassium tablets (argentometric titration)
•Experiment 4: Gravimetric determination of chloride in KCL tablet
•Experiment 5: Oxidation reduction titration of iron supplement (ferrous sulphate tablet)
•Experiment 6: Complexometric titration of calcium supplement tablet with EDTA
•Experiment 7: Potentiometric titration of aspirin tablet
•Experiment 8: Titration of a diprotic acid (maleic acid), identifying an unknown
•Experiment 9: Analysis of commercial vitamin C tablets using iodometric titration
•Experiment 10: Non-aqueous titration of Loratadine

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Objectives:

To master the principle and the implementation of the

potassium permanganate titration to ferrous sulphate tablet.

Intended learning outcomes (ILOs):

- describe the principle of redox titration

- determine the mass percentage of iron (II) in a common iron
supplement sample (ferrous sulphate tablets) using potassium
permanganate KMnO4 as a titrant in acidic conditions 3
Redox titrations:

Redox titrations are based on the transfer of electrons between

the titrant and the analyte.

These types of titrations are usually followed by potentiometry,

although dyes which change color when oxidized by excess
titrant may also be used.

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 A species undergoes oxidation when a loss of
electrons occurs.
 Substance undergoes reduction when it gains
electrons.
 These two processes always occur simultaneously
because there must be a transfer of electrons from one
species to another.
 Reducing agent is itself always oxidized and its own
oxidation number is always increased.

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Xn  Xn+1 + e- (Oxidation reaction) loss of es.

Ym+ e-  Ym-1 (Reduction reaction) gain of es.

Xn + Ym  Xn+1 + Ym-1 (Coupled Redox reaction)

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Analysis of Iron Tablets:

 Iron is a mineral that is essential to the human body.

 Iron plays a key role in the making of red blood cells, it
is one of the constituents of haemoglobin, the oxygen-
carrying agent in the blood.
 Iron is normally taken from food.
 Nevertheless, it is sometimes necessary to supplement
the iron through ‘iron tablets’
 Iron tablets found in the pharmacy usually contain iron
(II) sulphate (ferrous sulphate).
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Permanganate ion (MnO4-) is a deep purple color (oxidized form); while the
mangenous ion (Mn2+) is a pale pink color (reduced form). Actually, (Mn2+) is
colorless in acidic medium. As, the titration proceeds, the MnO4– will converted
to Mn2+ and simultaneously Fe2+ will converted to Fe3+. When whole of the
reducing agent (Fe2+) will consumed, the oxidizing agent (MnO4–) cannot be
reduced, then the addition even one drop of KMnO4 solution given its color to
the solution. This indicates the end point of the titration.

Thus permanganate titrations can be used as an indicator of redox rxns to

determine iron II:

MnO4- + 8H+ + 5e-  Mn2+ + 4H2O (Reduction reaction)

(deep purple) (pale pink)
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 KMnO4 is a widely used powerful oxidizing agent.
 It is readily available, cheap, and no indicator is
required unless very diluted solutions are used.
 KMnO4 is not a primary standard.
 A maximum quantitative action of KMnO4 is
obtained in presence of free H2SO4 (acidic
conditions).

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The unbalanced net ionic equation for the reaction:

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 Balancing redox reactions

Fe+2(aq) + MnO4-(aq) Mn+2(aq) + Fe+3(aq)

Oxidation half:
Fe+2(aq) Fe+3(aq) + 1e-
Reduction half:
MnO4-(aq) Mn+2(aq)
Balancing atoms:
Balancing
oxygens: MnO4-(aq)+ Mn+2(aq) + 4H2O
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 Balancing redox reactions
Balancing hydrogens:
Reaction happening in an acidic medium

MnO4-(aq)+8H+ Mn+2(aq) + 4H2O

Oxidation
numbers: Mn = +7, Mn = +2
O = -2

Balancing electrons:
The left side of the equation has 5 less electrons than the right side

MnO4-(aq)+8H++ 5e- Mn+2(aq) + 4H2O

Reduction Half 12
 Balancing redox reactions
Making the number of electrons equal in both half reactions

[Fe+2(aq) Fe+3(aq) + 1e- ]× 5

[MnO4-(aq)+8H++ 5e- Mn+2(aq) + 4H2O]×1

5Fe+2(aq) 5Fe+3(aq) + 5e-

MnO4-(aq)+8H++ 5e- Mn+2(aq) + 4H2O
5Fe2++MnO4-(aq)+8H++ 5e-
5Fe3+ +Mn+2(aq) + 4H2O + 5e- 13
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 Balancing redox reactions
5Fe2++MnO4-(aq)+8H+ 5Fe3+ +Mn+2(aq) + 4H2O

5 Fe 2+ ions are oxidized by 1 MnO4- ion to 5 Fe3+

ions. Conversely 1 MnO4- is reduced by 5 Fe2+ ions
to Mn2+.
If we talk in terms of moles:

5 moles of Fe 2+ ions are oxidized by 1mole of MnO4-

ions to 5 moles of Fe3+ ions. Conversely 1 mole of MnO4-
ions is reduced by 5 moles of Fe2+ ions to 1 mole of
Mn2+ ions. 15
 Conclusion from the balanced
chemical equation
For one mole of MnO4- to completely react with Fe2+, you will
need 5 moles of Fe2+ ions.
So, if the moles of MnO4- used up in the reaction is known,
then the moles of Fe2+ involved in the reaction will be 5 times
the moles of MnO4-

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Procedure:
1. Weigh accurately 20 tablets of iron supplement (Ferrograde folic) to find
out the average weight of one tablet.
2. Crush the tablets in the mortar and pestle.
3. Accurately weigh 0.3g sample of the crushed tablets.
4. Dissolve the sample in 20 ml of distilled H2O.
5. Add 30 ml of 1M Sulfuric acid (H2SO4) to the solution.
6. Titrate with 0.01M KMnO4 potassium manganate (VII) solution
(potassium permanganate). The end point for this reaction is light pink.
Make sure the color stays for 30 seconds without changing.
7. Calculate the weight of iron in each tablet.
8. Compare it to the manufacturer's claim statement.
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 Problem with KMnO4

The permanganate solution, once prepared, begins to decompose

as in the following reaction:

4 MnO4-(aq) + 2 H2O(l)  4 MnO2(s) + 3 O2(g) + 4 OH-(aq)

So, we need a solution whose concentration is precisely known

to be able to find the precise concentration of KMnO4 solution.

Standardization of KMnO4 solution with sodium oxalate

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 Vinitial
Vfinal- Vinital= Vused (in mL)

KMnO4 Important requirement:

The concentration of
Vfinal KMnO4 should be
known precisely

End point:
Pale Permanent
Pink color

250mL 250mL
250mL

Vused (in mL) 1L

VKMnO4 Used (in L)   19
1 1000mL
Calculations:
The balanced ionic equation for the reaction of Fe2+ ions
and MnO4- ions in acid solution is as follows:
1MnO4- + 5Fe2+ + 8H+  Mn2+ + 5Fe3+ + 4H2O
At equivalent point  # moles of MnO4- = # 5 moles of Fe2+
++
5 mole Fe +
2
= M MnO4 x V ml x ( ) x Awt Fe
% FeII 1 mole MnO4
x 100
Wt sample in (mgs)

+
𝐀𝐭𝐨𝐦𝐢𝐜 𝐰𝐭 𝐨𝐟 𝐅𝐞𝟐 𝐢𝐫𝐨𝐧 = 𝟓𝟓. 𝟖𝟒𝟕 𝐠/𝐦𝐨𝐥𝐞
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