Experiment Analysis of Iron in steel

Problem definition Mechanical properties of steel depend on its composition. Hence its
analysis is important for its use in industry.
Methodology Potentiometric method using K2Cr2O7as oxidizing agent to oxidize
Fe(II) in steel to Fe(III) facilitating its estimation.
Solution Estimation of percentage of iron in different steel samples.
Student learning Students will learn to perform
outcomes a)Potentiometric method
b)Composition of iron in different grades of steel

Principle:
Potassium dichromate oxidizes ferrous ion to ferric ion in the presence of acid as per the
reaction:
5Fe+2 → 5Fe+3 + 5e
MnO4- + 8H+ + 5e → Mn2+ + 4H2O_
5Fe+2 + MnO4- + 8H+ → 5Fe+3 + Mn2+ + 4H2O
The electrode potential (oxidation potential) in the titration depends upon the concentration of
Fe2+, Fe3+ and hydrogen ions. To avoid the effect of the change in the hydrogen ion
concentration, the titration is usually carried out in large excess of an acid. The oxidation
potential of this redox system is given by
RT Fe 3
E  E0  ln( 2 )
nF Fe
Connecting the redox electrode (Platinum) with a saturated calomel electrode (SCE)
completes the necessary cell as indicated below:
HgHg2Cl2 (s), Saturated KCl Fe3+, Fe2+Pt
(SCE)
When potassium dichromate is added Fe2+ is oxidised to Fe3+ whose concentration increases
with progressive addition of potassium permanganate. The observed EMF gradually
increases. At the end point, there will be a sharp increase due to sudden removal of all Fe 2+
ions. Plot between EMF measured (E) Vs. Volume of potassium permanganate added and
another plot between  E /V vs. Average volume of potassium permanganate are made. The
end point of the titration is measured graphically.
Requirements:
Reagents and solutions: 100 mL of K2Cr2O7 solution, 100 mL of steel solution, 2.0 N
H2SO4.
Apparatus: Calomel electrode, Platinum electrode, Potentiometer, Volumetric flasks,
Burette, Pipette, Beakers.
Procedure:
Calibration of Potentiometer: Switch on the potentiometer and connect the standard cell
terminals to either channel A (move channel switch to position A) or channel B (move the
channel switch to position B). The meter should read 1.018 V. In case it is not 1.018 V, adjust
the std. knob to obtain reference value.

Estimation of Fe(II) in steel: Transfer the given unknown steel [containing Fe(II)] solution
into a clean 100 mL standard flask and make the solution up to the mark with distilled water
and mix well. Pipette out 20 mL made up steel sample solution into a clean 100 mL beaker.
Add one test tube dilute sulphuric acid (2.0 N). Place Pt electrode in the beaker and connect
to the +ve terminal of the potentiometer. In another beaker, place 50 mL of saturated KCl
solution and dip the SCE in the solution and connect to the -ve terminal of the potentiometer.
Place a salt bridge to complete the cell. Read the EMF of the cell and note down the value.
Add 1 mL of K2Cr2O7 solution from a burette to the beaker containing steel sample solution.
Stir the solution carefully and measure the EMF. Continue the addition of K2Cr2O7 solution
and record the EMF for every 1 mL addition as per procedure till the potential shows a
tendency to increase rapidly. After the abrupt change in cell EMF is observed, continue the
titration to take 5 more reading by adding 1 mL burette solution every time. Plot
EMF(ordinate) vs. volume of K2Cr2O7added (abscissa) to get S-shaped curve which will
indicate the volumes between whish the end point lies.

Carry out another titration in similar way but by adding 1 mL aliquots of KMnO4 initially and
then 0.1 mL aliquots between the two volumes where the end point is detected. Continue the
titration beyond the end point as done above. The exact end point is determined by
differential method i.e. by plotting ΔE/ΔV vs. average volume of KMnO4 added. Calculate
the normality strength of the Fe(II) in the given solution.
Potentiometric Titration-I
Burette: Potassium dichromate solution (0.1 N)
Beaker: 20 mL of steel solution + one test tube dilute H2SO4
Electrodes: Indicator electrode (Pt) to red terminal and SCE to black terminal
Volume of
S. No. EMF (volts)
K2Cr2O7(mL)
1 0 -185
2 1 -125
3 2 -105
4 3 -90
5 4 -77
6 5 -64
7 6 -52
8 7 -37
9 8 -15
10 9 +48
11 10 +273

12 11 +274

13 12 +276

14 13 +278

15 14 +279
400

300

200

100

0
0 5 10
-100

-200

-300

EMF vs volume of KMnO4 added (mL)

Potentiometric Titration-II

Steel solution containing Fe(II) 20 mL + 20 mL (one test tube) 2.0 N H2SO4 in beaker,
K2Cr2O7 in burette
Vol. of
Sl. No. K2Cr2O7 EMF (Volt)
( mL)
1 7.3 018

2 7.5 20

3 7.7 23

4 7.9 27

5 8.1 31

6 8.3 35

7 8.5 40

8 8.7 43

9 8.9 48

10 9.1 54

11 9.3 64

12 9.5 76

13 9.7 100

14 9.9 115

15 10.1 140

16 10.3 143

17 10.5 147

18 10.7 152

19 10.9 154
 20 11.1 157

180
160
140
120
100
80 Series1

60
40
20
0
0 2 4 6 8 10 12

Figure II: Plot of plotting ΔE/ΔV versus average volume of K2Cr2O7 added.

Calculations:
By stoichiometry, 6 moles ofFe(II) will need 1 mole of K2Cr2O7 to complete oxidation.
Hence, 335.07 g Fe(II) will need 294.185 g of K2Cr2O7
Therefore, 1 mL K2Cr2O7 will oxidize 335.07/294.185= mg of Fe(II)

Volume of K2Cr2O7 consumed for oxidizing 20 mL of steel solution = V mL (Taken from

the second graph)
Therefore, Fe(II) present in the 20 mL steel solution = V x 1.7669 mg = X mg

This Fe(II) is present in 20 mL of steel solution given which contains Y mg/mLof steel.

Therefore, % Fe(II) in the steel sample = X x 100

Y

Result

Percentage of Fe (II) in the given steel sample =