Experiment no.

06

Determination of Ferrous Iron by a Standard Potassium

Dichromate Solution

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 Objectives

Main objective: Determination of amount of ferrous iron present in a given aqueous

solution by redox titration

Learning goals:

1. Preparation of standard K2Cr2O7 solution

2. Calculation of redox titration curves using Nernst
equation
3. Detection of end point in redox titration using redox
indicator

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 Theory: Chemistry behind the experiment

Oxidation-reduction reactions involve exchange of electrons between the

reacting substances in this volumetric analysis of Fe2+ using Cr2O72-

E° = 0.56 V

The above reaction is called as redox reaction because it could be represented

by two half reactions involving oxidation and reduction, respectively.

E˚ = -0.77V E˚ = 1.33V

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 Redox Indicator

Oxidation Reduction Indicator :

The change in potential at equivalence point of a titration may be detected by the
addition of a suitable indicator. An indicator that exhibits a change in colour
corresponding to a change in oxidation state is known as redox indicator.

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 Redox Indicator

The Nernst equation for this half-reaction is:

The indicator’s color changes from that of Inox to that of Inred when the ratio
[In ]red/[In ]ox changes from 0.1 to 10, then the end point occurs when the
solution’s potential is within the range

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 Redox titration Curve

➢ Diphenylamine: 1% solution in conc.

H2SO4 is used. The range of
diphenylamine Eind = 0.76 ± 0.059/2.
Between potential 0.73V-0.79V the color of
the solution changes gradually from
colorless to blue -violet
➢ E0 of Fe3+/Fe2+ (0.77V) and E0 of
diphenylamine (0.76V) are very close.
Phosphoric acid is added to remove Fe3+
from solution by forming [FeHPO4]+ and
reduces E0 of Fe2+/Fe3+ system, therefore,
prevents the premature oxidation of the
indicator.
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 Redox titration Curve

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 Chemicals & Apparatus

Chemicals Apparatus
• Mohr salt [(NH4)2Fe(SO4)2·6H2O] • Analytical Balance
solution • Volumetric flask
• 2N H2SO4 • Conical flask
• Conc. Phosphoric acid • Burette
• Dry K2Cr2O7 • Pipette
• Diphenyl amine solution • Measuring Cylinder (5mL, 50mL)
• DI water • Pipette filler
• Funnel

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 Making N/10 K2Cr2O7 solution

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 Experiment

Take 10 mL of the supplied

iron (Mohr's salt) solution in a
conical flask using a pipette

Mohr salt solution

Add 50 mL 2N sulfuric acid

Then add 4-5 drops of
and 5 mL of conc. Phosphoric
diphenyl amine indicator
acid

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 Experiment

Titrate slowly against standard until the addition of one drop

Potassium Dichromate solution causes the formation of
dropwise maintaining an interval intense purple or violet blue
of few seconds between each drop coloration

Cr3+ ion fives the green color

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 Data Table
Table #1
Title: Determination of volume of standard K2Cr2O7 solution required to titrate
10mL Mohr salt solution

No. of Volume of Burette reading (b.r.) Volume of K2Cr2O7 Average vol.

observations Mohr salt (f.b.r. ̶ i.b.r.) mL of K2Cr2O7
mL initial b.r. final b.r. mL
01 10 0.10 9.90 X
02 10 9.90 19.60
03 10 19.60 29.3

Difference should be with in ±0.1 mL.

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 Calculations
Concentration of potassium dichromate: Y N; Volume of the pipet used,volume (Fe): 10 mL
Average vol. of K2Cr2O7: X mL

Mass Ferrous iron: From the Redox reaction equation of Ferrous iron with potassium dichromate,
6 moles Fe(NH4)2(SO4)2.6H2O are equivalent to 1 mole K2Cr2O7 .

we can use the following relation to estimate the amount of iron (Fe2+) present in 1Litre of given
solution:

1 mL IN K2Cr2O7  0.05585 g Fe2+

X mL YN K2Cr2O7  (0.05585 × X × Y) g Fe2+ in 10 mL Mohr salt solution

Therefore, 1L supplied Mohr salt solution contains:

Result: Supplied Mohr salt solution contains Z g / L of Fe2+

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 Discussions

Percentage of Errors:

Known Value - Observed value

% of error =  100
Known value

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 Calculation (contd), Result and Discussion

Discussion: Should be based on-

➢ Precautions taken to minimize error
➢ Justification of error (despite sufficient precautions)
➢ Justification of error should be based on reasons that are
beyond your control

This the end of experiment

Submit your complete report before next experiment with
answer of supplied questions

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 Questions
➢ Prepare your report highlighting:
➢ Role of Fe in our daily life (Biochemical role, structural material, machine tools and
cookware) and importance of knowing the Fe content in a sample
➢ Redox half-reactions, reaction spontaneity and potential at the equivalence point.
➢ Theoretical background of the experiment
➢ Role of H3PO4 in the experiment
➢ The way diphenylamine acts as an indicator
➢ Step-by-step calculation of the experimental result
➢ Discussion with justification of error

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