INORGANIC CHEMISTRY-II CHM351 (LAB)
MANAL NASIR
SP23-BCH-014
ASSIGNMENT: 02
To: Dr. ABDUL RAHIM
Redox Titration Method for Determining Oxidizing Agents Using Potassium
Iodate (KIO₃)
1. Introduction
Redox titration is a type of volumetric analysis based on an oxidation-reduction reaction
between the analyte and titrant. It involves the transfer of electrons from a reducing agent
to an oxidizing agent. One of the most common oxidizing agents used in redox titrations is
potassium iodate (KIO₃), which acts as a primary standard due to its high purity, stability,
and known composition.
Potassium iodate is often used to determine the concentration of reducing agents such as
sodium thiosulfate, ferrous ions, and ascorbic acid through iodometric titration.
2. Principle of the Method
When potassium iodate reacts in an acidic medium with potassium iodide (KI), it liberates
iodine (I₂) in stoichiometric proportion.
The liberated iodine can then be titrated with a standard solution of a reducing agent such
as sodium thiosulfate (Na₂S₂O₃) until the endpoint is reached.
The reactions involved are:
At the endpoint, all iodine is reduced to iodide ions, indicated by the disappearance of the
blue color (starch–iodine complex).
3. Objective
To determine the amount or concentration of an oxidizing agent using potassium iodate as
a standard solution through redox titration.
4. Chemicals and Apparatus
Chemicals:
Potassium iodate (KIO₃), primary standard
Potassium iodide (KI)
Sulfuric acid (H₂SO₄), 1 M
Sodium thiosulfate (Na₂S₂O₃), standard solution (~0.1 M)
Starch indicator (freshly prepared 1%)
Apparatus:
Burette
Pipette (25 mL)
Conical flask (250 mL)
Volumetric flask (250 mL)
Funnel
Measuring cylinder
Wash bottle
Redox Titration Setup
5. Procedure
Step 1: Preparation of Standard Potassium Iodate Solution
Weigh accurately 0.3567 g of KIO₃ and dissolve it in distilled water.
Transfer to a 250 mL volumetric flask and make up to the mark with distilled water.
This gives a 0.01 M KIO₃ solution.
Step 2: Liberation of Iodine
Pipette 25.0 mL of standard KIO₃ solution into a conical flask.
Add about 2 g of KI and 10 mL of 1 M H₂SO₄.
The solution becomes brownish-yellow due to liberated iodine.
Step 3: Titration
Fill the burette with standard sodium thiosulfate solution.
Titrate the liberated iodine until the color changes from brown to pale yellow.
Add 2–3 drops of starch indicator, which turns the solution deep blue.
Continue titration dropwise until the blue color disappears, indicating the endpoint.
Step 4: Repeat
Repeat the titration to obtain three concordant readings (within ±0.1 mL).
6. Reaction Stoichiometry
From the equations:
Thus,
1 mole of KIO₃ reacts with 6 moles of Na₂S₂O₃.
7. Calculations
Let:
Using this formula, the exact molarity of sodium thiosulfate (or another reducing agent) can
be calculated.
8. Example Calculation
9. Indicators
The starch indicator is used because it forms a deep blue complex with iodine, which
disappears sharply at the endpoint.
However, it should only be added when the solution becomes pale yellow, as adding it too
early can cause the complex to become unstable.
10. Sources of Error
1. Addition of starch too early.
2. Incomplete mixing of solutions.
3. Light exposure causing decomposition of iodine.
4. Air oxidation of iodide ions before titration.
5. Impure or moist reagents.
11. Precautions
Always prepare starch solution freshly.
Keep the solution protected from light.
Use pure dry KIO₃ as it is a primary standard.
Rinse burette and pipette with respective solutions before use.
Perform titration carefully near the endpoint.
12. Applications
Standardization of sodium thiosulfate solution.
Determination of oxidizing agents like Cu²⁺, Fe³⁺, ClO₃⁻, and BrO₃⁻.
Used in food and pharmaceutical analysis.
Determination of chlorine content in bleaching powder and iodine in iodized salt.
13. Conclusion
The redox titration using potassium iodate is a precise and reliable method for determining
the strength of oxidizing or reducing agents. Potassium iodate, being a primary standard,
ensures high accuracy in volumetric analysis. The iodine liberated during the reaction serves
as an intermediate oxidant, allowing indirect but sharp titrations using starch as an
indicator.
15. References
1. Vogel, A.I., Textbook of Quantitative Chemical Analysis, 6th Ed., Pearson Education,
2000.
2. Harris, D.C., Quantitative Chemical Analysis, 9th Ed., W. H. Freeman, 2016.
3. Skoog, D.A., West, D.M., Holler, F.J., Fundamentals of Analytical Chemistry, 8th Ed.,
Cengage Learning, 2004.
4. IUPAC Compendium of Chemical Terminology, 2nd Ed. (1997).
5. Research Article: Zhao et al., Analytical Chemistry, 2020, 92 (15), 10112–10119.