KWAME NKRUMAH UNIVERSITY OF SCIENCE AND

TECHNOLOGY

COLLEGE OF ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING

TITLE: ESTIMATION OF “AVAILABLE CHLORINE” IN

BLEACHING POWDER

NAME: AMUAH PRINCE NICHOLAS

COURSE: BSC. PETROCHEMICAL ENGINEERING
YEAR: SECOND YEAR
EXPERIMENT NO. : A.1.2.1.
I.D. NO: 7666512
DEMONSTRATOR: ADOLF-OTI BOAKYE
DATE: 5TH MARCH 2014.
Aims and Objectives:
1. To determine the amount of chlorine in bleaching powder using titrimetric analysis.
2. . To learn how to use the electronic balance to weigh the mass of substances.

INTRODUCTION
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.
Chlorine, deriving its name from the Greek word “chloros”, meaning pale green, is one of the
halogens in Group 1 7 (VIIa) of the periodic table. With an atomic number of 17, it was
discovered by a Swedish chemist named Carl Wilhem Scheele, who thought it was a
compound, until 1810 when a British chemist named Sir Humphry Davy proved that it was a
compound and hence gave it its name. Chlorine at ordinary temperatures is a greenish-yellow
gas that can be liquefied under a pressure of 5170torr at 20 0C. It has an irritating odour which
is very dangerous in large concentrations. Free chloride doesn’t occur in nature, but its
compounds are common minerals.
The method of bleaching, originally done by exposure to the Sun was first practiced during
ancient and medieval times in Egypt, China, etc. the powerful bleaching properties of
chlorine was discovered in 1785 by French chemist Claude Louis Berthollet. Bleaching
powder is a mixture containing Calcium hypochlorite [CaOCl2] as the active bleaching agent.
It was the standard bleaching powder until about 1925 when the use of liquefied chlorine
replaced it

Chlorine plays an important biological role in the human body, where the chloride ion is the
principal anion in intracellular and extracellular fluids. Chlorine in bleaching powder can also
be used as disinfectants to help improve sanitation by means of it being used to scrub algae
from gutters and damp wall surfaces, pulp bleaching. Chlorine in large quantities is used to
produce insecticides, such as DDT. It is widely used as an industrial bleaching agent of paper
and textiles. Ordinary household laundry bleach contains the active ingredient sodium
hypochlorite, 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.
In the determination of the available chlorine, two methods are us. 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

The second method would involve the titration of the hypochlorite solution or suspension
against standard arsenite solution; it is done best when the excess of the arsenite solution is
added and then back titrated 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 H 2SO4. 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

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

PROCEDURE

a) 2.0g of bleaching was weighed accurately and transferred into a beaker and mixed
with water and stirred for some time.
b) It was transferred quantitatively into 250ml volumetric flask and made up to the mark
with 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/ml
1 2 3
Final 15.90 31.20 46.10
Initial 1.10 15.90 31.20
Titre Value 14.80 15.30 14.90

CALCULATION

For the first titration

[Na2S2O3] = 0.40M
V (Na2S2O3) = 14.80ml = 0.0148dm3
n (Na2S2O3) = c[Na2S2O3] x v(Na2S2O3)
= 0.40 x 0.0148
=5.92x 10-3mol

n (I2) =1
n(Na2S2O3) 2

n(I2) = n(Na2S2O3)
2
=5.92 x103mol
2
=2.96 x10-3mol

But n(I2) = n(Cl2)

∴ n(Cl2) = 2.96 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 2.96 x 10-3
50
= 0.0148mol
⇒mass (Cl2) = n(Cl2) x M(Cl2)
But molar mass of chlorine =35.5 x2
=71
= 0.0148 x 71
= 1.0508g

For the second titration

[Na2S2O3] = 0.40M
V(Na2S2O3) = 15.30 = 0.0153dm3
n(Na2S2O3) = [Na2S2O3] x v(Na2S2O3)
= 0.40 x 0.0153
=6.12 x 10-3mol
n(I2) = n(Na2S2O3)
2
 = 3.06x 10-3mol

But n(I2) = n(Cl2)

∴ n(Cl2) = 3.06 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 3.06 x 10-3
50
= 0.0153mol
⇒m (Cl2) = n(Cl2) x M(Cl2)
= 0.0153 x 71
= 1.086g

For the third titration

[Na2S2O3] = 0.40M
V(Na2S2O3) = 14.90ml =0.0149dm3
n(Na2S2O3) = [Na2S2O3] x v(Na2S2O3)
= 0.40 x 0.0149
=5.96 x 10-3mol

n(I2) = n(Na2S2O3)
2
= 2.98 x 10-3mol
But n(I2) = n(Cl2)
∴ n(Cl2) =2.98 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 2.98 x 10-3
50
= 0.0149mol
⇒m (Cl2) = n (Cl2) x M(Cl2)
= 0.0149 x 71
= 1.058g

The mean mass, x = 1.051+1.086+1.056

3
= 1.065g

Mass,(X) Mean mass(x) (X-x) (X-x)2

1.051 1.065 -1.4 x10-3 1.96 x 10-6
1.086 1.065 2.1x10-3 4.41 x 10-6
1.058 1.065 -7.0 x10-3 4.9 x 10-5
∑ f ( x−x)2 = 5.54 x 10 -5

√
2
∑ f ( x −x )
Standard deviation (S) = n
Where n = 3 and f = 1

= √ 5 . 54x10-5

= 4.297 x 10-3
3

S
×100 %
Relative standard deviation = X
-3
4 . 297 x 10
×100 %
= 1 . 065
= 0.403%
x
×100 %
m
Percentage of Cl2 in sample = t
mt = mass of sample
1.065
×100 %
= 2.5
= 42.6%

DISCUSSION

From the above experiment, we realise that series of colours are observed when various
reagents are reacted; a brown colour for the reaction between Potassium Iodide and Sodium
thiosulphate and a brownish-black colour when the resulting solution was reacted with
Sulphuric Acid, a light yellow colour when titrated with the turbid solution and a colourless
solution when starch indicator was added to the solution and finally titrated.

Also, the reaction between the bleaching powder and the sulphuric acid produced gaseous
chlorine hence the addition of the potassium iodide to avert the escape of the chlorine. This is
because it forms a salt when reacted with the potassium iodide. However in this state, the
amount of available chlorine cannot be determined thus the titration of turbid solution against
hypo solution. This enables us to determine the number of moles of iodide which in turn
enable us to determine the available chlorine in the sample.

The ability 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. This is accounts for why the titration
was allowed to proceed to certain point before the starch indicator was added. The sulphuric
acid and the sodium thiosulphate acted as oxidising and reducing agents respectively to
enhance the occurrence of the various reactions.

The titre values obtained from the titration are 14.80ml, 15.30ml, and 14.90ml respectively.
This trend of values follows that the values obtained are consistent titre values looking at how
they differ from each other by a slight difference of about 0.1ml. The standard deviation of
the data collected was found to be equal to 4.297 x 10-3, a value which by far less than one
(1) implying that the average mass of chlorine in the sample calculated was very close to the
true mass. The magnitude of the relative (percentage) standard deviation determined shows
that the calculated mass only deviated from the actual mass by a percentage of 0.403%.
On the other hand, the percentage mass of chlorine in the 42.6% inferring that almost half of
the bleaching powder contains chlorine.

CONCLUSION

From the above experiment, we can conclude that the marginal values of the relative standard
deviation and the percentage mass shows that the average mass of chlorine in the sample is a
true reflection of its true mass.
Also, the percentage mass of the chlorine being about half the content of the bleaching
powder indicates that the chlorine forms a great portion of the bleaching powder unlike a
normal percentage of 20% to 30%.
In a nut shell, the method used in determining the available chlorine was fruitful.

PRECAUTIONS

1. All fragile glassware was carefully handled.

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

REFERNECES

 Modern Inorganic Chemistry, Alan G Sharpe and Catherine Housecraft, 4th Edition,
Pages 468-480.
 Inorganic Chemistry, P.A. Cox, 2nd Edition, Pages 177-180