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Iodometry (1) - Read-Only

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Estimation of Iodine in Iodized Common Salt

Iodine is an essential element for life and one of the heaviest elements required by living organisms.
However, around 1/3 of the world’s population lives in areas of iodine deficiency.

The
practice of adding iodine to salt is a safe,
easy and effective way of overcoming
iodine deficiency in our diet. Globally two
chemical forms of iodine are used for
iodization; Iodates (IO3-) and Iodides (I-).

The iodides degrade more readily in presence


of impurities, exposure to sunlight, moisture
and exposure to heat, whereas the iodates
remain stable under extremes of weather and
handling. USA uses potassium iodide (77
mg/Kg) while Germany and India use
potassium iodate (25-20 mg/Kg) for iodine
fortification.

www.consumeraffairs.in
www.hrt.org
Theoretical Background
The direct iodometric titration method called as iodimetry, refers to titrations with a
standard solution of iodine.

The indirect iodometric titration method, termed iodometry, deals with the titration
of iodine liberated in chemical reactions.

Experiment involves three steps:

 Determining whether iodate or iodide anion is present in the given salt sample
 Standardising a solution of sodium thiosulphate
 Estimating the amount of iodine in given by performing an iodometric titration
using the standardized sodium thiosulphate solution

Iodate anion

IO3-
Theoretical Background
Standard Solution: A solution for which the concentration is known accurately.
The process of determining the exact concentration of a solution is termed as standardization.
In a titration, it is critical to know the exact concentration of the titrant (the solution in the burette which will
be added to the unknown) in order to determine the concentration of solutions being tested.
Standardization of Sodium Thiosulfate
Sodium thiosulphate is titrated against a standard solution of copper sulphate.

2Cu2+ + 4I- Cu2I2 + I2

I2 + 2S2O32- S4O62- + 2I-

Net Reaction: 2Cu2+ + 2I- + 2S2O32- Cu2I2 + S4O62-


Estimation of Iodine

2 Na2S2O3 + I2 Na2S4O6 + 2 NaI

Test for Iodate


Iodate in presence of free hydrogen ion, oxidizes added iodide to give free iodine; which turns starch blue
IO3- + 5 I- +6 H+ 3 I 2 + 3 H2O

Test for Iodide


Iodide is oxidized to free iodine with an acidic solution of sodium nitrite. The free iodine turns starch blue
2 NaNO2 + H2SO4 2HNO2 + Na2SO4
2 HNO3 + 2 I- I 2 + 2 NO + H2O

Starch used as indicator for titrations with iodine


Theoretical Background
Indicator : starch

Starch-iodine complex has a strong colour; blue-purple-brown-grey-black


Starch binds very strongly to iodine (binds to the I 3- ion in solution)

We add starch when the iodine concentration is a little less because the starch-iodide complex
has less solubility and can stop iodine from reacting completely with thiosulphate
Some of the iodine may bind to copper in solution
To make sure that all iodine reacts with sodium thiosulphate, we add KSCN
KSCN binds to copper thereby releasing iodine and making it available to react

Solution containing Iodine Solution containing Starch-Iodine complex


Experimental Protocol
Test for iodate solution
Moisten ta pinch of salt with 2-3 drops of the given solution (mixture of A, D and E). If iodate is present the salt will turn
blue/grey and the color will be retained for several minutes before turning brown.

Test for iodide solution


Moisten a pinch of salt with 2-3 drops of the given solution (mixture of A, B and C). If iodide is present the salt will turn blue and
remain blue for several minutes before fading.

Determination of Iodate Content (if test A is positive)

1. Weigh X g of the given salt sample and transfer into a 250 mL conical flask and dissolve it in 50 mL water.
2. Add 1 mL 2N H2SO4 (use dropper, do not pipette by mouth), then add 5 mL of 10% KI solution using a measuring cylinder.
The solution will turn yellow. Wrap the mouth of conical flask with a piece of filter paper and keep it in cupboard for 10 minutes.
3. Take 60-80 mL solution of (approx.) 0.005 M Na 2S2O3 in a 250/500 mL plastic beaker and use for titration. Rinse burette and
fill it in and adjust zero level.
4. Remove flask from cupboard and titrate with Na 2S2O3 solution until the solution turns pale yellow. Now add approx. 10 drops
of starch indicator. The solution will turn dark purple. Continue titrating until the solution becomes colorless.
5. Record the volume of titrant (Na 2S2O3 solution) used and calculate the amount of iodine present in part per million (ppm).

Standardization of Sodium Thiosulfate

1. Pipette out 10 mL copper sulfate of concentration 0.005 M in a conical flask and add 5 mL of 5% KI solution. The solution will
turn yellow in color.
2. Titrate with Na2S2O3 solution until the solution turns pale yellow. Add 7-8 drops starch indicator solution at this stage.
3. Continue the titration until the purple color fades, then add 5-6 drops of KSCN solution and titrate again. The end point gives
a colorless solution.

CAUTION: To ensure that you have obtained the true end point, stir the flask for 20 seconds and then wait for 20 seconds to
make sure that the purple color does not reappear.

4. Repeat the titration to get concordant readings. Calculate the molarity of the given sodium thiosulfate solution.
Observations and Calculations
Standardization of Sodium Thiosulfate

S. No. Volume of sodium thiosulphate used


from the burette
1 9.4 mL
2 9.5 mL
3 9.5 mL

Given concentration of copper sulphate = 0.005 M

Equivalents of Copper = Equivalents of Thiosulphate

(Normality x Volume) of Copper = (Normality x Volume) of Thiosulphate

0.005 x 10 mL = Normality of Thiosulphate x Volume of Thiosulphate (Burette Reading)

Suppose Burette Reading is 9.5 mL


Normality of Thiosulphate = (0.005 x 10)/9.5
Normality of Thiosulphate = 0.0053 M
Observations and Calculations
Estimation of Iodine
S. No. Volume of sodium thiosulphate used
from the burette
1 2.4 mL
2 2.5 mL
3 2.5 mL

IO3- + 6S2O32- + 6H+ 3S4O62- + I- + 3H2O

Consider the above reaction of iodate ions present in salt sample reacting with sodium thiosulphate

6 x M1V1 Iodate = M2V2 Thiosulphate


6 x M1 x 50 = 0.0053 x Burette Reading

Value obtained by standardizing sodium thiosulphate against a standard copper


solution

Suppose Burette Reading is 2.5 mL


6 x M1 x 50 = 0.0053 x 2.5
Molarity of Iodate solution = 4.4 exp -6
Observations and Calculations
Thus, the solution contains 4.4 exp -6 moles of Iodine per Liter of solution
The solution contains 4.4 exp -6 x 126.90 grams Iodine per Liter of solution
Atomic Weight of Iodine = 126.90 g

Solution contains 5.6 exp -3 grams Iodine per Liter of solution


= 5.6 mg of Iodine per Liter of solution

Concentration in ppm

To report in ppm

Suppose we started with 10 g of salt,

10 g salt was dissolved in 50 mL of water

In 50 ml of solution;

(5.6 mg x 50)/ 1000 = 0.28 mg of Iodine

Thus, 0.28 mg of Iodine in 10 g of salt

ppm means parts per million; which is mg per Kg

(0.28/10) x 1000 = 28 ppm of Iodine was present in our salt sample


Results
 Iodate anions were identified in the given salt sample

 Concentration of iodate ions and iodine was determined by performing an iodometric titration

 Concentration of Iodine in given salt sample = 28 ppm

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