2/8/2021

ExpErimEnt no. 2
Object:- To determine the strength of given
unknown ferrous ammonium sulphate solution by
titrating against standard K2Cr2O7 using potassium
ferricyanide as an external indicator

Principle: -
The oxidizing agent K2Cr2O7 in presence of dil. H2SO4 gives three atoms of nascent oxygen [O]

K2Cr2O7 + 4 H2SO4 K2SO4 + Cr2 (SO4)3 + 4 H2O + 3 [O]

The liberated [O] oxidizes ferrous ion (Fe+2) to ferric ion (Fe+3)
6 FeSO4 + 3 H2SO4 + 3 [O] 3 Fe2 (SO4)3 + 3 H2O
The complete reaction is:
6 [FeSO4.(NH4)2SO4.6H2O] + K2Cr2O7 + 7 H2SO4
3 Fe2(SO4)3 + K2SO4 + Cr2(SO4)3 + 6 (NH4)2SO4 + 43 H2O
Or ionically,
Cr2O7-2 + 14 H+ + 6 Fe+2 2 Cr+3 + 6 Fe+3 + 7 H2O

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2 K3Fe(CN)6 + 3 FeSO4 Fe3[Fe(CN)6]2 + 3K2SO4

Ferro ferricyanide
(Dark blue complex)
Usually at the end point (all Fe+2 ions are oxidized to Fe+3) the color of the
indicators drop becomes light brownish yellow due to reaction of indicator
with Fe+3 ions to produce brown colored ferric ferricyanide complex.
Fe2(SO4)3 + 2K3[Fe(CN)6] 3K2SO4 +2Fe[Fe(CN)6]
Ferric ferricyanide
Brownish yellow
Thus, at the end point, the indicator fails to produce blue color when treated
with a drop of titration mixture
• Reagents: Ferrous ammonium sulphate solution, N/40 potassium
dichromate solution, 0.1 % solution of potassium ferricyanide, dil.
Sulphuric acid.
• Apparatus: Burette, pipettes, conical flask, glass rod, funnel, white glazed
tile, test tubes

Procedure:
Standardization of K2Cr2O7 solution:
• Wash all the apparatus with distilled water.
• Rinse and fill the burette with N/40 K2Cr2O7 solution.
• Pipette out 10 ml of FAS solution (N/40) in a clean conical flask and add 5 ml of dil.
H2SO4.
• Put a series of drops of indicator (potassium ferricyanide solution) with the help of glass
rod on a white tile.
• Titrate the FAS solution against K2Cr2O7 solution.
• Near end point, take a drop of titration mixture and put it on one of indicators drops on
tile and see the color.
• A strong blue color will be produced. Continue the titrations and repeat the process at
different intervals and when the color of indicator drop does not give blue color, the end
point is reached.
• Note the reading of the burette and repeat the titration until two concordant readings
are obtained.

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Estimation of FAS:
• Wash all the apparatus with distilled water.
• Rinse and fill the burette with K2Cr2O7 solution.
• Pipette out 10 ml of unknown FAS solution in a clean conical flask and add 5 ml of dil.
H2SO4.
• Put a series of drops of indicator (potassiumferricyanide solution) with the help of glass
rod on a white tile.
• Titrate the FAS solution against K2Cr2O7 solution.
• Near end point, take a drop of titration mixture and put it on one of indicators drops on
tile and see the color.
• A strong blue color will be produced. Continue the titrations and repeat the process at
different intervals and when the color of indicator drop does not give blue color, the end
point is reached.
• Note the reading of the burette and repeat the titration until two concordant readings
are obtained.

Observation Tables:
Standardization of K2Cr2O7 solution:
Sr. No. Volume of Burette Volume of Concordant
FAS taken Readings (ml) K2Cr2O7 Reading(ml)
(ml) Initial Final consumed (ml)

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Estimation of FAS
Sr. No. Volume of Burette Volume of Concordant
FAS taken (ml) Readings (ml) K2Cr2O7
Initial Final consumed Reading(ml)
(ml)

Calculations:
Standardization of K2Cr2O7 solution:
• N1V1 = N2V2
•
• N1 = Normality of ferrous ammonium sulphate solution (N/40)
• V1 = Volume of ferrous ammonium sulphate solution
• N2 = Normality of potassium dichromate solution
• V2 = Volume of potassium dichromate solution
•
• N2 = N1V1/V2
•
• N2 = ------------N

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• Estimation of FAS
N3V3 = N4V4
N3 = Normality of ferrous ammonium sulphate solution
V3 = Volume of ferrous ammonium sulphate solution
N4 = N2 = Normality of potassium dichromate solution
V4 = Volume of potassium dichromate solution
N3 = N4V4/V3
N3 = -----------N
Strength = N3 × Equivalent weight of FAS
= N3 × 392
= -------------gm./L

• Result:
• The strength of given unknown ferrous ammonium
sulphate solution = ----------- g/L
• Precautions:
• Potassium dichromate acts as an oxidizing agent in
acidic medium, add some dil. H2SO4.
• End point should be observed carefully

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