KWAME NKRUMAH UNIVERSITY OF SCIENCE AND TECHNOLOGY

COLLEGE OF ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING

TITLE: ESTIMATION OF CHLORINE WITH AgNO3 (MOHR’S

METHOD)

NAME: AMPAW-ASIEDU,MERCY
COURSE: BSC. CHEMICAL ENGINEERING
YEAR: SECOND YEAR
EXPERIMENT NO. : A.1.2.3.
I.D. NO: 3643609
T.A.: ASANTE NNURO WILLIAM
DATE: 9TH FEBRUARY, 2011.
Aims and Objectives:
To determine the weight and percentage of the “available chlorine’ in bleaching powder using titrimetric
analysis.

INTRODUCTION
Although chlorine is one of the most widely distributed elements,its discovery is of relatively recent date. A
Swedish chemist, Scheele, is given credit for its discovery. It is a heavy green coloured gas, and of very
corrosive properties. It attacks violently excretal and organic bodies. It is soluble in water and gives a greenish
solution of irritating smell, and soon disposes, especially when exposed to light. The gas can be liquefied by
compressing it in special machines, and is kept and transported in strong steel cylinders.

Chlorine plays an important biological role in the human body, where the chloride ion is the principal anion in
intracellular and extracellular fluids. Chlorine is widely used as an industrial bleaching agent of paper and
textiles. Ordinary household laundry bleach contains the active ingredient sodium hypochlorite (about 5 percent
of masses), which is prepared by reacting chlorine gas with a cold solution of sodium hydroxide:

Cl2(g) + NaOH(aq)  NaCl(aq) + NaClO(aq) + H2O(l)

Chlorine is also used to purify water and disinfect swimming pools. When chlorine dissolves in water, it
undergoes the following reaction:

Cl2(g) + H2O(l)  HCl(aq) + HClO(aq)

It is thought that the ClO- ions destroy bacteria by oxidizing life-sustaining compounds within them.
Chlorinated methanes, such as carbon tetrachloride and chloroform, are useful organic solvents. Large
quantities of chlorine are used to produce insecticides, such as DDT. However, in view of the damage they
cause on the environment, the use of many of these compounds is either totally banned or greatly restricted.
Chlorine is also used to produce polymers such as polyvinyl chloride.

Calcium chlorohypochloride (bleaching powder), a white crystalline solid, which consist mainly of
Ca(OCl)2,CaCl2 and slake lime [Ca(OH)2]. The key is the hypochlorite which determines the bleaching action.
By reacting chlorine gas with cold slaked lime, bleaching powder is usually prepared.

Ca(OH)2(aq) + Cl2(g)  Ca(OCl)Cl(aq) + H2O(l)

Cl2 is liberated upon the treatment of bleaching powder with HCl

OCl-(aq) + Cl-(aq) + 2H+(aq)  Cl2(aq) + H2O(l)

Cl2 also known as the available chlorine is liberated by the action of the acid and is expressed as percentage by
the weight of the bleaching powder.
As an aim of this experiment, available chlorine in bleaching powder would be determined by treating a
suspension of the powder with KI and H2SO4. The liberated chlorine will set free from the KI an equivalent
amount of iodine which is titrated against a standard thiosulphate solution.

CHEMICALS AND INSTRUMENTS USED

 Dilute 4N H2SO4.
 KI.
 Hypo solution.(0.5M)
  250ml volumetric flask.
 Pipette.
 Burette.
 Retort stand.
 Conical flask.
 Electronic balance.
 Porcelain dish
 Starch indicator.
 Bleaching powder.
 Measuring cylinder.

PROCEDURE

TABLE OF VALUES

Burette
Readings/cm3 1 2 3
Final 9.30 18.80 28.20
Initial 0.00 9.30 18.80
Titre Value 9.30 9.50 9.40

Average titre =
[Na2S2O3] = 0.50M
First titre value
V(Na2S2O3) = 9.30cm3
n(Na2S2O3) = [Na2S2O3] x V (Na2S2O3)
=
= 0.00465mol
n(I2) = x n(Na2S2O3)
= 0.002325mol
but n(I2) = n(Cl2)
∴ n(Cl2) = 0.002325mol
This amount is contained in 50cm3 of the turbid solution.
∴ The amount of Cl2 in the 250cm3 turbid solution is
=
= 0.011625mol
⇒m(Cl2) = n(Cl2) x M(Cl2)
= 0.011625x 71
= 0.825g
Second titre value

[Na2S2O3] = 0.50M
V(Na2S2O3) = 9.50cm3
n(Na2S2O3) = [Na2S2O3] x V(Na2S2O3)
=
= 0.00475mol
n(I2) = x n(Na2S2O3)
= 0.002375mol
but n(I2) = n(Cl2)
∴ n(Cl2) = 0.002375mol
This amount is contained in 50cm3 of the turbid solution.
∴ The amount of Cl2 in the 250cm3 turbid solution is
=
= 0.011875mol
⇒m(Cl2) = n(Cl2) x M(Cl2)
= 0.011875 x 71
= 0.843g

Third titre value

[Na2S2O3] = 0.50M
V(Na2S2O3) = 9.40cm3
n(Na2S2O3) = [Na2S2O3] x V(Na2S2O3)
=
= 0.00470mol
n(I2) = x n(Na2S2O3)
= 0.002350mol
but n(I2) = n(Cl2)
∴ n(Cl2) = 0.002350mol
This amount is contained in 50cm3 of the turbid solution.
∴ The amount of Cl2 in the 250cm3 turbid solution is
=
= 0.01175mol
⇒m(Cl2) = n(Cl2) x M(Cl2)
= 0.01175 x 71
= 0.834g

The mean mass M =

= 0.834g
 X M (X-M) (X-M)2
0.825 0.834 -0.009 81 x 10-6
0.843 0.834 0.009 81 x 10-6
0.834 0.834 0.000 0.000

= 162 x 10-6

Standard deviation (S) =

=
= 7.348 x 10-3
Relative standard deviation =

=
= 0.88%
Percentage of Cl2 in sample =
mt = mass of sample
=
= 33.36%

DISCUSSION
It can be inferred from the definition of density that density is directly proportional the mass of the substance
but inversely proportional to its volume. Thus as mass increases, density increases and as volume increases,
density decreases. It was observed that the wooden objects were less dense than water.
After comparing the averages of experimental densities to the graphical densities were about the same. The
graph was a scattered graph and thus a line of best fit was drawn for each graph.
Aims and Objectives:
1. To determine the amount of chlorine in bleaching powder using titrimetric analysis.
2.

INTRODUCTION
Although chlorine is one of the most widely distributed elements, yet its discovery is of relatively recent date.
The famous Swedish chemist, Scheele, is given credit for its discovery. It is a heavy gas green color, and of
very corrosive properties. It attacks violently organic bodies. It is soluble in water and gives a greenish solution
of irritating smell, and soon disposes, especially when exposed to light. The gas can be liquefied by
compressing it in special machines, and is kept and transported in strong steel cylinders.

Chlorine plays an important biological role in the human body, where the chloride ion is the principal anion in
intracellular and extracellular fluids. Large quantities of chlorine are used to produce insecticides, such as DDT
Chlorine is widely used as an industrial bleaching agent of paper and textiles. Ordinary household laundry
bleach contains the active ingredient sodium hypochlorite (about 5 percent of masses), which is prepared by
reacting chlorine gas with a cold solution of sodium hydroxide:

Cl2(g) + NaOH(aq)  NaCl(aq) + NaClO(aq) + H2O(l)

Calcium chlorohypochloride (bleaching powder), a white crystalline solid, which consist mainly of
Ca(OCl)2,CaCl2 and slake lime [Ca(OH)2]. The active component is the hypochlorite which is responsible for
the bleaching action. By reacting chlorine gas with cold slaked lime, bleaching powder is usually prepared.

Ca(OH)2(aq) + Cl2(g)  Ca(OCl)Cl(aq) + H2O(l)

Cl2 is liberated upon the treatment of bleaching powder with HCl

OCl-(aq) + Cl-(aq) + 2H+(aq)  Cl2(aq) + H2O(l)

The available chlorine refers to the chlorine liberated by the action of the dilute acids on the hypochlorite and is
expressed as a percentage by weight in the case of bleaching powder. Commercial bleaching powder contains
36-38 percent of available chlorine.

Two methods are in common use for the determination of the available chlorine. In the first, the hypochlorite
solution or the suspension is treated with an excess of a solution of potassium iodide, and strongly acidified
with acetic acid:
OCl- + 2l- + 2H+  Cl- + l2 + H2O
The liberated iodine is titrated with standard sodium thiosulphate solution. The solution should not be strongly
acidified with hydrochloric acid, for the little calcium chlorate which is usually present, by virtue of the
decomposition of the hypochlorite, will react slowly and react with potassium iodide and liberate iodine:
ClO3- + 6l- + 6H+  Cl- + 3l2 + 3H2O

In the second method, the hypochlorite solution or suspension is titrated against standard arsenite solution; this
is best done by adding the excess of the arsenite solution and then back titrating with the standard iodine
solution.

In this experiment, the first method would be used. Available chlorine in bleaching powder would be
determined by treating a suspension of the powder with KI and H2SO4. The liberated chlorine will set free from
the KI an equivalent amount of iodine which is titrated against a standard thiosulphate solution.

CHEMICALS AND EQUIPMENT

 Dilute 4N H2SO4.
 KI.
 Hypo solution.
 500ml volumetric flask.
 Pipette.
 Burette.
 Retort stand.
 Conical flask.
 Electronic balance.
 Starch indicator.
 Bleaching powder.
 Measuring cylinder.

PROCEDURE

Procedure Observation
a) 2.5g of bleaching was weighed accurately and
transferred into a beaker and made into a paste.
 b) It was transferred quantitatively into 250ml A turbid solution of bleaching powder was
volumetric flask and made up to the mark with obtained
distilled water and shaken well.
c) A burette was rinsed and filled with a standard
hypo solution, taking note of the initial burette
reading.
d) 50ml of the turbid solution was pipetted with
into a 250ml conical flask; adding 2g of KI and
then 15ml of 4N H2SO4 ,
e) It was mixed well and the mouth covered with
watch glass and titrated with hypo solution.
f) When only a deep yellow colour remained, 2ml
of 1% of freshly prepared starch was added and
there was continuous addition of hypo solution
drop by drop with shaking until the blue colour
just disappeared.
g) The titration procedure was repeated to get two
concordant values.

TABLE OF VALUES

Burette
Readings/cm3 1 2 3
Final 23.90 38.60 44.40
Initial 9.60 24.10 30.00
End point for starch 24.10 38.80 44.60
Titre Value 14.5 14.7 14.6

Average titre = 14.5 + 14.7 + 14.6 = 14.6cm3

3
For the first titration

[Na2S2O3] = 0.50M
V(Na2S2O3) = 14.6cm3
n(Na2S2O3) = c[Na2S2O3] x v(Na2S2O3)
= 0.50 x 14.5
1000
=7 x 10-3mol
n(I2) = x n(Na2S2O3)
= 3.5 x 10-3mol
but n(I2) = n(Cl2)
∴ n(Cl2) = 3.5 x 10-3mol
This amount is contained in 50cm3 of the turbid solution.
∴ The amount of Cl2 in the 250cm3 turbid solution is
= 250 x 3.5 x 10-3
50
 = 0.0175mol
⇒m (Cl2) = n(Cl2) x M(Cl2)
= 0.0175 x 71
= 1.243g

For the second titration

[Na2S2O3] = 0.50M
V(Na2S2O3) = 14.7cm3
n(Na2S2O3) = c[Na2S2O3] x v(Na2S2O3)
= 0.50 x 14.7
1000
=7.35 x 10-3mol
n(I2) = x n(Na2S2O3)
= 3.675 x 10-3mol
but n(I2) = n(Cl2)
∴ n(Cl2) = 3.675 x 10-3mol
This amount is contained in 50cm3 of the turbid solution.
∴ The amount of Cl2 in the 250cm3 turbid solution is
= 250 x 3.675 x 10-3
50
= 0.018mol
⇒m (Cl2) = n(Cl2) x M(Cl2)
= 0.0184 x 71
= 1.306g

For the third titration

[Na2S2O3] = 0.50M
V(Na2S2O3) = 14.6cm3
n(Na2S2O3) = c[Na2S2O3] x v(Na2S2O3)
= 0.50 x 14.6
1000
=7.3 x 10-3mol
n(I2) = x n(Na2S2O3)
= 3.65 x 10-3mol
but n(I2) = n(Cl2)
∴ n(Cl2) = 3.65 x 10-3mol
This amount is contained in 50cm3 of the turbid solution.
∴ The amount of Cl2 in the 250cm3 turbid solution is
= 250 x 3.65 x 10-3
50
= 0.018mol
⇒m (Cl2) = n (Cl2) x M(Cl2)
= 0.0183 x 71
= 1.299g
The mean mass X = 1.243 + 1.306 + 1.299
3
= 1.283g

X X (X-X) (X-X)2
1.243 1.283 -0.040 1 x 10-6
1.306 1.283 0.023 5.29 x 10-4
1.299 1.283 0.016 2.56 x 10-4

= 7.83 x 10-4

Standard deviation (S) =

Where n = 3 and f = 1
=
= 0.016
Relative standard deviation =

=
= 1.25%
Percentage of Cl2 in sample =
mt = mass of sample
=
= 51.32%

b) Normality is the number of equivalents of a defined species per litre according to the specified reaction. In
this definition the number of hydrogen referred to may be replaced by the equivalent amount of electricity, or
by one equivalent of any other substance, but the reaction to which the definition is applied must be clearly
specified.

Normality = Number of equivalents

Number of L
Number of mill-equivalents
Number of mL

c) The concentration of 4N H2SO4 in moldm-3 is 4moldm-3 because

Concentration = Number of moles (equivalents)
Number of dm-3 (L)
Since 1L = 1000dm-3

DISCUSSION
When the bleaching powder was reacted with the sulphuric acid, the chlorine obtained was in the gaseous form
and so potassium iodide was immediately added to the product of the reaction to prevent the gaseous chlorine
from escaping. This is because it formed a salt when reacted with the potassium iodide. But in this state, the
chlorine available cannot be determined so the turbid solution is titrated against hypo solution. This enabled us
determine the number of moles of iodide which in turn enable us to determine the available chlorine in the
sample.
The nature of starch indicator to easily combine with iodine to form complex species was the reason why it was
not used at the start of the titration. That is why the titration was allowed to proceed to certain point before the
starch indicator was added.
The titre values obtained from the titration are 14.5cm3, 14.7cm3, and 14.6cm3 and this follows that they are
consistent titre values since they differ from each other by a difference of 0.1. The standard deviation of the data
collected was found to be equal to 0.016. This value is far less than 1; hence it implies the average mass of
chlorine in the sample calculated was very close to the true mass. The magnitude of the relative (percentage)
deviation determined shows that the calculated mass only deviated from the actual mass by a percentage of
1.25%.
The percentage mass of chlorine in the 51.32% which implies that half of the bleaching powder constituted
chlorine.
PRECAUTIONS
 Equipment was washed before and after each experiment.
 Bleaching powder solution was shaken well to form a turbid solution.
 The mass of KI and bleaching powder were accurately weighed.
 The burette readings were taken from below the meniscus.

CONCLUSION
Since the magnitude of the relative (percentage) deviation determined shows that the calculated mass only
deviated from the actual mass by a percentage of 1.25% and hence it can be concluded that the average mass of
chlorine in the sample calculated was very close to the true mass. The percentage mass of chlorine in the was
about half the content of bleaching powder. This indicates that chlorine forms a great portion of the bleaching
powder.
The method used in determining the available chlorine was successful.

REFERNECES
General Chemistry by Whitten D. Peck
Vogel’s Textbook of Quantitative Analysis (page 382-383)
Essential Chemistry by Raymond Chang (page 863)

PRECAUTIONS
 Equipment was washed before and after each experiment.
 Bleaching powder solution was shaken well to form a turbid solution.
 The mass of KI and bleaching powder were accurately weighed.
 The burette readings were taken from below the meniscus.

CONCLUSION
The determined percentage of chlorine is 33.36% of mass chlorine in the bleaching powder. This shows that
bleaching powder consist of an amount of chlorine. The reduction effect of Na2S2O3 makes it possible for the
estimation of available chlorine in bleaching powder.

REFERENCES
General Chemistry by Whitten D. Peck
General Chemistry by Raymond Chang
Lab. manual