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Vivek Raghubar


Analtyical Chemistry Practical Report #12,13

Wet Chemistry
Practical 12
Preparation and standardization of approximately 0.05M Na2S2o3 solution using KIO3

Redox titrations using sodium Thiosulphate as a reducing agent is known as
Iodometric titrations as they are used to titrate iodine specifically. The reaction
involved is:
I2 + 2Na2S2O3 2NaI + Na2S4O6
I2 + 2S2O32- 2I- + S4O6 2-
In the above equation I2 has been reduced to I-

The iodine/thiosulphate titration is a method for calculating the

molarity of the oxidising agent solution. A known volume of an oxidising
agent is added into an excess solution of acidified KI. The KI was acidified by the
addition of 2M H2SO4. From this reaction Iodine will be released.

The iodine that was released from the above reaction was titrated against a standard
thiosulphate solution.
From the stoichiometry of the reaction ( which can be seen below), the amount of iodine
can be determined. From this the concentration of the oxidising agent was calculated.

The over reaction is

From this reaction the ratio is 1:6

Starch is used in iodometric titrations as the indicator as this absorbs the Iodine
released in the titration. The absorption of Iodine caused the solution to change to a
dark blue/black colour. The starch indicator is only added to the conical flash containing
the iodine after the solution turns to a pale yellow from brown to avoid a complex
between the starch and iodine forming as this will affect the titration( equation below).
After the addition of the indicator the solution is titrated against the thiosulphate solution,
the iodine and thiosulphate react.

As the amount of iodine in the conical flask decreases, the dark blue/black colour fades.
This is the endpoint of the titration.

Table of reagents
Reagent Harzards
1. Solid Na2S2O3.5H2O
2. Solid KIO3 Oxidizing flame
3. 10% KI sol
4. 2M H2SO4 sol Corrosive
5. 1% starch sol

As stated in the practical manual. No changes were made.

0.05M approx. Na2S2O3.5H2O sol
C=n/v n=m/Mm C1V1=C2V2
Mm Na2S2O3.5H2O= 248.08g/mol
250ml solution to be made
n Na2S2O3.5H2O= 0.250L x 0.05
n Na2S2O3.5H2O= 0.0125M
m Na2S2O3.5H2O= 0.0125M x 248.08g/mol
m Na2S2O3.5H2O= 3.101g
Actual weighed mass = 3.08
Approx. 0.01M 100ml KIO3 sol
Mm KIO3 = 214.00g/mol
n KIO3 =0.01m x 0.1L
n KIO3 = 0.001mol
m KIO3 = 0.001mol x 214g/mol
m KIO3 =0.214g
Primary standard

Titration table thiosulphate vs potassium iodide

20ml aliquot of potassium iodide was used.
Thiosulphate volumes(ml)
Initial Final Actual volume
0.28 24.18 23.90
0.30 24.14 23.84
1.24 25.16 23.92

Average volume delivered =23.89ml

C Na2S2O3 = 6x 20.00mlx 0.01M /1x 23.89ml
c Na2S2O3 = 0.0502M

The concentration of thiosulphate was found to be 0.0502M.

Practical 13

Determination of the concentration of commercial pool chlorine as Ca(OCl)2

Bleach has become one of the leading house hold brands for everyday cleaning. The
power/effectiveness of bleach is directly related to its oxidizing strength. Detergents are
used to remove all sorts of grease and grime from all surfaces by emulsification action
and formation of a micelle which is assisted by agitation by adding physical heat/friction.
Most chlorine bleaches contain a hypochlorite ion OCl-. They are generally presented as
Na(OCl)2 or Ca(OCl)2. This experiment outlines how the use of redox reactions can be
used to determine the amount of oxidizing agents there is present in a liquid such as
Two redox reactions occur in this experiment

Form this reaction equation the ratio is 2 thiodulphate : 1 Iodine

Excess KI sol is added to the bleach oxidizing the I- ions to I2. The iodide that forms is
then titrated with thiosulphate solution that had been standardized in practical 12.
The indicator used is starch as this is also an iodimetry titration. The starch is again
added only after the solution in the conical flask turns to a pale yellow from brown to
avoid a complex between the iodine and starch forming. The end point is reached when
a single drop of thiosulphate turns the solution colourless.
Table of reagents
Reagent Harzards
1. Na2S2O3 standardized
2. Solid KIO3 iodate free Oxidizing flame
3. Commercial pool Corrosive
4. 2M H2SO4 sol Corrosive
5. Starch indicator

As stated in the practical manual. No changes were made.

The concentration of thiosulphate was found to be 0.0502M.

C=n/v n=m/Mm C1V1=C2V2

Ca(OCl)2 solution of 0.025M of 100ml
Mm= 142.98g/mol
n Ca(OCl)2 =0.025M x 0.1L
n Ca(OCl)2 = 0.0025mol
m Ca(OCl)2 = 0.0025mol x 142.98g/mol
m Ca(OCl)2 = 0.3575
Actual mass weighed = 0.5195g
Titration table of Bleach solution vs thiosulphate
20ml aliquots of bleach sol were taken for titration
Volumes of thiosulphate dispensed
Initial Final Actual volume
0.42 32.78 32.36
0.10 32.36 32.26
0.44 32.74 32.30

Average volume of thiosulphate= 32.30ml

Mol thiosulphate = mol Bleach sol
N thiosulphate = 0.0502M x 0.250L
N Bleach = 0.01255mol/2
= 0.006275mol
M Bleach = 0.006275 x 70.9g/mol
=0.4448g Cl
%Cl in sample = 0.4448g/0.5195g x 100
= 85.63%

Author unknown, 7th/04/2015
Practical manual