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Addis Ababa Institute of Technology

Chemical and Bio Engineering Department
Analytical chemistry lab report
Title Iodometric analysis
Group Members Id No.
1. Khalid Keno UGR/7794/12
2. Fuad Sadudin UGR/5321/12
3. Firealem Ashenafi UGR/0034/12
4.Fikru Gurmu UGR/4360/12

5 Zelalem

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Objective
To determine the concentration of oxygen in water

Theory
Analytical reactions using iodide ion as reducing agent are called Iodometry and procedures
using iodine as oxidizing agent are called iodimetry.

Iodometry is one the most important redox titration methods. Iodine reacts directly fast and
quantitatively with many organic and inorganic substances thanks to its relatively low PH
independent redox potential and reversibility of iodine iodide reaction.

In Iodometric titration the reduction of free iodine to iodide ion and oxidation of iodide ion to
free iodine occur.

In Iodometric titration an oxidizing agent is allowed to react with neutral or acidic medium with
the excess of KI to liberate free iodine.

KI + Oxidizing agent  I2

The free iodine is titrated against standard reducing agent usually with sodium thiosulfate.

Iodometry is commonly used to analyze the concentration of oxidizing agents in water solution.
For example, it can be used to determine the amount of dissolved oxygen in water. Oxygen
oxidizes iodide to iodine. Iodine dissolves in iodide containing solutions to give tri iodide ions,
which has a dark brown color. The tri iodide ion solution is then titrated against standard
thiosulfate solution to give iodide against starch indicator.

I3- + 2e-  3I- together with reduction potential of thiosulfate

S4O62- + 2e-  2S2O32-
The overall reaction is thus,
I3- + 2S2O32-  S4O62- + 3I-

For simplicity, the equations will usually be written in terms of aqueous molecular iodine rather
than tri iodide ion.

The disappearance of deep blue color due to the decomposition of iodine starch cultrate marks
the end point.

Generally, Iodometry can be used both to determine the amount of reducing agent by (direct
titration with iodine) and of oxidizing agent by (titration of iodine with thiosulfate).

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Materials Used
 Funnel
 Burette
 Pipette
 Conical flask
 Measuring cylinder
 Distilled water
 Electronic Scale
 Spatula
 NaHCO3
 K2Cr2O7
 KI
 HCl
 H2SO4
 Starch Solution
 Standard hypo solution
 Paper and Pencil

Procedure 1, Standardization of Hypo Solution

1. 20ml distilled water was added to a clean conical flask.
2. 0.5g NaHCO3 was measured using electronic scale.
3. The 0.5g NaHCO3 was added to into the flask which contains the 20ml distilled water.
4. Then, HCl was drop wisely added to flask using pipette until the reaction between HCl
and NaHCO3 reaches completion or bubble formation stops.
5. 5ml of 20% KI solution was measured using measuring cylinder and added to the flask.
6. 10ml of 0.0167M K2Cr2O7 solution was added to the conical flask.
7. Then, the mixture inside the flask was shaken.
8. Then the flask was covered with a watch glass and kept in dark place for 5 minutes.
9. The watch glass was rinsed with distilled water into the flask.
10. 50ml distilled water was added along the walls of the flask.
11. The mixture was titrated quickly against hypo solution from the burette until the dark
brown color changes to light yellow. The light yellow color was immediately changed to
light aqua color.
12. The volume of added hypo solution was recorded.
13. After this, 1ml of starch solution was dropped using pipette in to the flask containing
the mixture.
14. The titration process was continued until light aqua color disappears.

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 15. Finally, the amount of added hypo solution was recorded once again.
Procedure 2, Estimation of dissolved oxygen in water
1. 25ml of tap water was measured using measuring cylinder and added to a clean conical
flask.
2. 2g of potassium iodide, KI, was measured using electronic scale and added to the flak.
3. Then, 10 ml of 6M sulfuric acid was measured and added to the flask.
4. The observation was recorded.
5. Then, 1ml starch solution was added to the flask.
6. And the mixture inside the flask was titrated against the hypo solution until the yellow
solution color changes to light orange or “Shiro” color.
7. Finally, the amount of added hypo solution was recorded.

Data

Sub-Experiment 1, Standardization of Hypo solution

Chemicals Quantity Concentration Solution color

Distilled water 1 20ml Colorless
NaHCO3(s) 2g Colorless
HCl(aq) Few drops Colorless
KI(aq) 5ml 20% Colorless
K2Cr2O7 (aq) 10ml 0.0167M Dark brown
Distilled water 2 50ml Dark brown
Hypo solution 1 2.5ml Light yellow for short
period of time then to
aqua color
Starch (indicator) 1ml Aqua
Hypo solution 2 6.5ml Colorless

Sub-Experiment 2, Estimation of dissolved oxygen in water

Chemicals Quantity Concentration Solution color

Tap water 25ml Colorless
KI 2g Colorless
H2SO4 10ml 6M Yellow
Starch (indicator) 1ml Yellow
Hypo solution 2.5ml Light Orange or “Shiro”

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 Calculation

Sub-Experiment 1
Known

VHYPO = 2.5ml + 6.5ml = 9ml

VKI = 5ml

VK2CR2O7 = 10ml, CK2CR207 = 0.0167M

Required

CHYPO=?

Solution

Using the dilution law,

VHYPO*CHYPO = VIODINE*CIODINE

But, VIODINE = VKI + VK2CR2O7 = 5ml + 10ml = 15ml

CIODINE = 0.5CKI = 0.33CK2CR207 = 0.33*0.0167M = 0.0056M

Then, CHYPO = (VIODINE*CIODINE)/VHYPO = (15ml*0.0056M)/9ml = 0.0093M

CHYPO = 0.0093M * 2 = 0.0186N

Sub-Experiment 2
Known

CHYPO = 0.0093M

VHYPO = 2.5ml, VO2 = VH20 + VH2SO4= 25ml + 10ml = 35ml

Required

CO2 =?

Solution

Using the dilution law,

CO2 = (CHYPO *VHYPO)/VO2 = (0.0093M *25ml)/35ml = 0.00663M = 0.00663 mole/liter

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1mole of oxygen contains 32g of oxygen, and then 0.00663 moles of oxygen contain 0.212g of
oxygen. Hence we have 0.212mg of oxygen in each ml of sample.

Discussion and Conclusion

Water is a great source of oxygen for living things such as sea weeds and fishes. The
concentration of oxygen in water determines the living condition of plants and animals.
Similarly, the concentration of oxygen in a sample determines the rate of reactions which
depend on the amount of oxygen, especially redox reactions. Thus, it is vital to determine the
concentration of oxygen in a sample, for example water.

In Iodometric titration free iodine is used since it is difficult to prepare a solution of iodine
(iodine sublimates and is less soluble in water) and it is dissolved in KI solution.

KI + I2  I3

During titration the starch indicator should be added after the iodine solution fades to straw
yellow color as early addition of starch indicator at high iodine concentrations would result in
irreversible precipitation of the iodine starch complex.

In this experiment, HCl and H2SO4 were used to provide acidic medium to oxidizing agent.

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