Estimation of Ferric Ion and Ferrous Ion by Using

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The document discusses methods to estimate ferrous and ferric ions in water samples using titrimetric and potentiometric techniques.

Titrimetric and potentiometric methods were used to estimate ferrous and ferric ions. Titrimetric analysis involved titrating against potassium dichromate solution. Potentiometric analysis used potentiometry without indicators.

The titrimetric method involves a simple acidification step to decompose iron complexes into free Fe2+ and Fe3+ ions. The amounts of free iron are then determined by titrating against potassium dichromate solution using an oxidation-reduction reaction.

University of central Punjab campus Phalia

Course: Applied Chemistry Lab

Topic:Estimation of ferric ion and ferrous ion


by using redox titration

Submitted to: Nimra Meer

Submitted by: Sawera Bibi


Estimation of ferric ion and ferrous ion by using redox titration

Theory:
Titrimetic and potentiometric methods were employed for the analysis of the ions of iron (ferrous
and ferric ) in natural water samples. The method for the determination of iron employs a simple
acidification step in order to decompose iron hydroxide and iron-complexes into free iron, Fe(III)
and Fe(II). The amounts of free iron were detected titrimetrically and electroanalytically .Titrimetric
analysis was done using using potassium dichromate wherein an oxidation reduction reaction was
involved. Indicator used was diphenyl amine. The electro analytical technique used was
potentiometry. Potentiometric analysis did not require the use of any indicators.It was concluded
from the present study that potentiometric analysis was more accurate and less time consuming
and the results obtained were reproducible

Apparatus:

 100 ml standard flask,


 Burette,
 250 ml Conical Flask,
 20 ml Pipette,
 Funnel
 Simple balance with Fractional weights.

Chemicals Required:

 Potassium dichromate (K2Cr2O7 )


 stannous chloride (SnCl2)
 Syrupy phosphoric acid (H3PO4 )
 Diphenylamine
 Ferrous iron solution & distilled water

Principle:
The method for determination of iron involved a simple acidification step in order to decompose
iron hydroxide and iron complexes into free iron Fe3+ and Fe2+. The amounts of iron
were determined titrimetrically and electroanalytically.

Methodology:
Titrimetry :
Ferrous iron in the sample waters is estimated by titrating against standard K2Cr2O7 solution in acid
medium using diphenyl amine as the indicator . In order to estimate the ferric iron , all of it , is first
reduced to the ferrous state with the help of stannous chloride.

2Fe3+(aq) + Sn2+(aq) ------------ 2Fe2+(aq) + Sn4+(aq)


While reducing the ferric iron , a slight excess of stannous chloride is added to ensue complete
reduction .The excess unreacted SnCl2 is removed by the addition of mercuric chloride which
oxidizes stannous chloride to stanic chloride.
SnCl2 + 2HgCl2 ---------------- SnCl4 + Hg2Cl2

Since mercurous chloride is not acted upon by the oxidants used for the titration it is allowed to
remain in the solution . After reduction , the solution containing the ferrous iron present originally
and the ferrous iron obtained by the reduction of ferric iron is titrated against K2Cr2O7 solution
and the total amount of Fe2+ iron is calculated.
Amount of Fe3+ iron = Amount of total Fe2+ iron –amount of Fe2+ iron originally present.

Estimation of Ferrous iron :


The sample water containing the ions of iron was titrated against potassium dichromate in the
presence of acid mixture ( H2SO4 and H3PO4 ) . The indicator used was diphenyl amine. The results
are tabulated in Table-1 and the amount of ferrous ion was calculated.

Estimation of ferric iron:


Reduction of ferrous to ferric iron
5 ml of conc. HCl was added to the sample water and the contents were heated to boiling. stannous
chloride was added dropwise till the yellow colour due to Fe3+ ion just disappeared. The solution
was cooled and 10 ml of a saturated solution of mercuric chloride was added with stirring to
remove excess of SnCl2. A silky white precipitate of Hg2Cl2 was formed upon the addition of HgCl2.
The solution was discarded when a black or grey or no precipitate was formed and the process was
repeated. The sample water was now titrated against potassium dichromate in the presence of acid
mixture (H2SO4 and H3PO4 )diphenyl amine indicator. The results are shown in Table-2

Observation:

Titrimetry:
Estimation of ferrous iron:
Table 1
Burette reading
Volume of
S.No. FAS (Total Fe )2+
K2Cr2O7run
Initial reading Final reading down

1 20 0.0 3.2 3.2

Estimation of ferric iron:


Table 2
Burette reading
Volume of
S.No. Vol. of mixture K2Cr2O7run
Initial reading Final reading down

1 20 0.0 8.8 8.8


Estimation of ferrous:
K2Cr2O7 FAS
M1=0.022 M2=?
V1= 3.2 V2 = 20
n1= 1 n2=6
M2=(M1V1/n1)*(n2 /V2)= 0.021
Amount of Fe2+ = W1 =M2 * 56/10=0.118 gm/100 ml

Estimation of ferric:
K2Cr2O7 FAS (Total Fe2+)
M1=0.022 M3=?
V1= 8.8 V3 = 20
n1= 1 n3=6
M3=(M1V1/n1)*(n3 /V3)=0.058
Amount of Fe2+ =W1 = M2*56/10=0.118.gm/100 ml
Amount of total Fe2+ =W2=M3*56/10= 0.325 gm/100ml
Amount of Fe3+ =W2-W1 =0.207 gm/100 ml

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