Total Residual Chlorine by Titration

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Determination of Total Residual Chlorine by Titration (Iodometric Method)

Principle:

Chlorine will liberate free iodine from potassium iodide solutions at pH 8 or less. The
liberated iodine is titrated with a standard solution of sodium thiosulfate with starch as
indicator. The titration is done at pH 3 to 4 to avoid partial oxidation of thiosulfate to
sulfate. The minimum detectable concentration approximates 40 ppb Cl 2 if 0.01N titrant
is used with a 1000 mL sample.

Apparatus:

 Beaker
 Stirring Rod
 Burette
 Pipette
 Graduated Cylinder
 Aspirator
 Volumetric Flasks

Reagents:

 Glacial Acetic Acid


 Potassium Iodide
 Concentrated Sulfuric Acid
 0.1 N Sodium Thiosulfate Stock Solution
 0.005 N Potassium Iodate Solution
 0.005 N Standard Sodium Thiosulphate Solution
 Starch Indicator Solution

Preparation of Reagents:

0.1 N Sodium Thiosulfate Stock Solution

Dissolve 25 g of sodium thiosulphate in 1 L pre-boiled distilled water.

0.005 N Standard Sodium Thiosulfate Solution

Dilute 50 mL of 0.1 N Sodium Thiosulfate Stock Solution in a 1 L volumetric flask. Store


at least two weeks before standardization.

.005 N Potassium Iodate Solution

Dry .1784 g potassium iodate crystals in an oven at 103oC for 1 hour. Place in a
dessicator to cool at room temperature. Dissolve in 1 L distilled water.

Starch Indicator Solution


Weigh 1 g potato starch and 5 mg mercuric iodide, then add cold water to make a
paste. Boil 100 mL distilled water and add the paste. Continue to boil while stirring
until a thin, translucent fluid is obtained. Cool to room temperature before use.

Standardization of 0.005 N Sodium Thiosulphate Stock Solution

1. To 80 mL of distilled water, add 1 mL concentrated sulfuric acid, 5 mL potassium


iodate solution and 1 g potassium iodide crystals.
2. Titrate with sodium thiosulphate solution until pale yellow.
3. Add 1 mL of starch indicator solution.
4. Continue titrating until blue color disappears.
5. Calculate the concentration of sodium thiosulphate using this formula:

1
𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑑𝑖𝑢𝑚 𝑡ℎ𝑖𝑜𝑠𝑢𝑙𝑝ℎ𝑎𝑡𝑒 𝑐𝑜𝑛𝑠𝑢𝑚𝑒𝑑, 𝑚𝐿

Procedure:

1. Pipette 5 mL glacial acetic acid and 1 g potassium iodide crystals in a beaker.


2. Add the sample in the beaker and mix.
3. Titrate with 0.005 N standard sodium thiosulphate until pale yellow.
4. Add 1 mL starch indicator solution.
5. Continue titrating until blue color disappears.
6. Calculate the total residual chlorine using the formula below:

𝐶𝑙2 𝐴 𝑥 𝑁 𝑥 35450
𝑚𝑔 𝐶𝑙 𝑎𝑠 =
𝐿 𝑚𝐿 𝑠𝑎𝑚𝑝𝑙𝑒
where:

A = volume of sodium thiosulphate, mL


N = normality of sodium thiosulphate

Reference:

Standard Methods for the Examination of Water and Wastewater Part 4500 Cl B.

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