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8 IODOMETRIC DETERMINATION
OF AVAILABLE CHLORINE IN A
SAMPLE OF BLEACHING POWDER
Structure
8.1 Introduction
Objectives
8.2 Principle
8.3 Requirements
8.4 Solutions Provided
8.5 Procedure
8.6 Observations and Calculations
8.7 Result
8.1 INTRODUCTION
In the previous experiment you learnt about and performed iodimetric determination
of ascorbic acid in a tablet of Vitamin C. In this process we recalled from Unit 10 of
the Basic Analytical Chemistry course (Section 10.7.1) that the I2/2I‒ couple is of
medium oxidising power.Molecular iodine is a weak oxidant, whereas the iodide ions
are relatively weak reductant. Accordingly, the I2/I– redox couple can be used for the
determination of reductants as well as the oxidants. In the previous experiment you
used I2 (generated in situ from acidification of KIO3) as the oxidizing agent to
determine the reductant, ascorbic acid. In the present experiment you will be using
iodide ions (from KI) to determine available chlorine in bleaching powder. Such a
determination wherein iodide ions are used as a reducing agent is termed as
iodometric determination.
Due to this deterioration, a sample of bleaching powder may always contain lesser
amount of chlorine than expected and therefore a sample of bleaching powder needs to
be analysed for its effective or available chlorine. In the next experiment you would
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learn about precipitation titrations and perform a precipitation titration for the
determination of chloride ions in a solution.
8.2 OBJECTIVES
After studying and performing the experiment, you should be able to:
• define available chlorine,
• define iodometric titrations,
• state and explain the principle of iodometric titrations with reference to the
determination of available chlorine in a sample of bleaching powder,
• state the reasons for using acetic acid to liberate chlorine from bleaching
powder,
• prepare a standard solution of potassium dichromate and use it to standradise a
solution of sodium thiosulphate,
• write the chemical equations involved in the titration of a solution of bleaching
powder solution with sodium thiosulphate,
• prepare a solution of bleaching powder from the given sample,
• perform the determination of available chlorine in the solution of bleaching
powder, and
• calculate the amount of available chlorine in the solution of bleaching powder.
8.3 PRINCIPLE
As mentioned in the introduction, a sample of bleaching powder liberates chlorine gas
(Cl2) on treatment with glacial acetic acid, as per the following reaction.
Ca (OCI2 ) + 2CH3 COOH → Ca(CH 3COO)2 + H 2 O + CI 2 …(8.1)
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The standradisation of sodium thiosulphate by using potassium dichromate is also
based on iodimetric titrations. The reaction between potassium dichromate and sodium
thiosulphate is mediated through the participation of iodide ions provided by
potassium iodide as explained below.
In acidic medium, Cr2O72- ions gets reduced to Cr (III) ions as per the following
equation
Cr2 O 72− + 14H+ + 6e- → 2Cr 3+ + 7H 2 O …(8.6)
The iodide ions from KI on the other hand can get oxidised to I2 as follows:
2I − → I 2 + 2e − …(8.7)
In order to maintain the electron balance, we can multiply equation 8.7 by 3 to get the
following,
6I − → 3I 2 + 6e − … (8.8)
Adding equations 8.6 and 8.8, we get the overall ionic equation for the reaction
between potassium dichromate and potassium iodide as :
Cr2 O 72− + 14H + + 6I − → 2Cr 3+ + 3I 2 + 7H 2 O … (8.9)
Thus, from Eq. 8.9, one mole of potassium dichromate reacts with 6 moles of
potassium iodide and liberates 3 moles of iodine in the process.
The liberated iodine, in turn, reacts with sodium thiosulphate solution as per the
following equation
3I 2 + 6S2 O 32− = 6I − + 3S4 O 62− …(8.10 )
The iodide ions are regenerated back. The net chemical reaction involving a titration
of potassium dichromate and sodium thiosulphate in the presence of excess potassium
iodide can be written by combining Eq. 8.8 and Eq. 8.9, as shown below,
Cr2 O 72− + 14H + + 6I − → 2Cr 3+ + 3I 2 + 7H 2 O ... (8.9)
We see from Eq. 8.11 that one mole of potassium dichromate is equivalent to 6 moles
of sodium thiosulphate. Therefore, the molarities are related by the following
relationship.
6 MDichromateVDichromate = MThiosulphateVThiosulphate … (8.12)
You would be using this equation to compute the molarity of the given solution of
sodium thiosulphate.
8.4 REQUIREMENTS
Apparatus Chemicals
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Volumetric flask (100 cm3) –1 Bleaching powder
3
Burette (50 cm ) –1 Potassium dichromate
3
Pipette (10 cm ) –1 Potassium iodide
Weighing bottle –1 Sodium thiosulphate
Burette stand with clamp –1 Sodium carbonate
3
Conical flasks (100 cm ) –2 Sulphuric acid
Funnel –1 Sodium bicarbonate
3
Beakers (250 cm ) –2 Acetic acid
Starch
8.6 PROCEDURE
The determination of available chlorine in a sample of bleaching powder using
iodometric titration consists of the following steps:
a) Preparation of potassium dichromate primary standard
b) Standradisation of sodium thiosulphate solution
c) Preparation of the solution of the bleaching powder sample
d) Determination of available chlorine in the above solution by iodimetric
titration
Follow the instructions given below in sequential manner
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• Pipette out 10 cm3 of potassium dichromate solution in a 100 cm3 conical Sodiu
flask, add 10 cm3 of dilute sulphuric acid and 1 g sodium hydrogen carbon
carbonate with gentle swirling to liberate carbon dioxide. an atm
CO2 i
• Add 10 cm3 of 10% KI solution, swirl, cover the flask with watch glass which
and allow the solution to stand for about 5 minutes in a dark place. air an
oxidat
• Titrate the liberated iodine against the sodium thiosulphate solution taken from a
in the burette until the solution acquires a light pale yellow colour.
• Repeat the standardization procedure at least three times and record your
observations in Observation Table 8.1.
• Add a little more water, triturate with the pestle and allow the mixture to
settle.
• Grind the residue with a little more water, and repeat the operation until
the whole of the sample has been transferred to the flask either in solution
or in a state of very fine suspension, and the mortar washed quite clean.
• Make the volume upto the mark by adding more distilled water.
• Wash the burette with distilled water and rinse with standard solution of
sodium thiosulphate and then fill the burette with the same.
• Add about 10 cm3 of 10% potassium iodide (KI) solution and about half
test tube of glacial acetic acid to the flask.
• Titrate the liberated iodine against the sodium thiosulphate solution taken
in the burette until the solution acquires a light pale yellow colour.
• Repeat the standardization procedure at least three times and record your
observations in Observation Table 8.2.
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a) Preparation of standard solution of potassium dichromate
Mass of weighing bottle + potassium dichromate = m1 g = ..............g
Mass of weighing bottle (after transferring potassium dichromate)
= m2 g = .............. g
Amount of potassium dichromate transferred = m1 – m2 = m g = ............. g
Molar mass (Mm) of potassium dichromate = 294.18 g mol−1
Volume of potassium dichromate prepared = 100 cm3
Molarity of standard potassium dichromate solution =
m × 1000 10m
M K Cr = = = ...........M
2 2O 7 100 × 294.2 294.2
6 M DichromateVDichromate
M Thiosulphate =
VThiosulphate
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Mass of bleaching powder taken =
The molarity of the iodine liberated from KI solution (which in turn is equal to the
amount of chlorine liberated from the bleaching powder on the action of acetic acid)
can be determined as follows.
8.8 RESULTS
The available chlorine (the grams of chlorine liberated from 100 g of the bleaching
powder on treatment with dilute acid) = ….. g
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