Estimation of Aniline by Bromination Method

2.
Estimation of Aniline by Bromination Method
Date:
Aim:
To estimate the amount of aniline present in whole of the given solution by
bromination method.
Principle:
Aniline and some of the derivatives having the free ortho and para position can be
estimated by bromination method. The method involves the following steps,
(a) Bromination of aniline by bromination mixture:
Aniline reacts with bromine to form 2,4,6- tribromoaniline. Since the yield is
quantitative, it is used for the estimation of aniline. The bromine required is obtained by
treating a mixture of potassium bromide and potassium bromate with dilute
hydrochloric acid. The bromine so liberated reacts with aniline to produce
tribromoaniline while excess of bromine remains unreacted.
5 KBr + KBrO3 + 6 HCl 3 Br2 + 3 H2O + 6 KCl
(b) Determination of unreacted bromine:
The unreactive bromine is treated with potassium iodide, the equivalent iodine
thus liberated is determined iodometrically with sodium thiosulphate solution using
starch as indicator.
Br2 + 2 KI 2 KBr + I2
2 Na2S2O3 + I2 2 NaI + Na2S4O6

Sodium tetrathionate
Procedure:
Preparation of standard potassium dichromate solution
The standard potassium dichromate solution can be prepared by weighing
accurately about 1.2260 g (0.016 M) of potassium dichromate, dissolving in water and
making up to 250 ml in a standard measuring flask.
Standardization of sodium thiosulphate solution
Into a 250 ml iodine flask, pipette 20 ml of standard potassium dichromate
solution. Add 10 ml of 1 M sulphuric acid and 1 g of sodium hydrogen carbonate into
the iodine flask with gentle swirling. Then add 0.5 g of potassium iodide and swirl the
flask and closed the flask, allow the solution to stand for 5 minutes in a dark place.
Titrate against sodium thiosulphate solution taken in the burette, until a light pale
yellow color is obtained. Add 1 ml of starch solution and continue the titration till the
blue color of starch-iodide complex disappears. Repeat the titration to get at least two
concordant readings.
Blank titration
Pipette out 20 ml of brominating solution in a 250 ml iodine flask and 5 ml of
concentrated hydrochloric acid and add 0.5 g of KI and immediately insert the stopper.
Keep the solution in dark 10 – 15 minutes. Wash the stopper and walls of the flask with 5
ml of water. Titrate this with sodium thiosulphate solution until the solution acquires
light yellow color and then add 5 – 6 drops of starch solution and continue the titration
with sodium thiosulphate solution. At the end point blue color disappears. Note the
reading of thiosulphate solution required (A). Repeat the titration to get at least two
concordant readings.
Estimation of Aniline:
The given solution dissolve in water and made up the volume to 100 ml. 20 ml of
this solution was pipetted out into a 250 ml iodine flask and add 5 ml of concentrated
hydrochloric acid. Brominating mixture is now added to this solution till it achieves
light yellow color and then 0.5 g of KI is added and immediately insert the stopper.
Keep the solution in dark 10 – 15 minutes. Wash the stopper and walls of the flask with 5
ml of water. Add 10 ml of chloroform shakes vigorously and titrate the liberated iodine
with sodium thiosulphate using starch solution as indicator. The end point is blue color
of starch-iodine complex disappears. Note the reading of thiosulphate solution required
(B). Repeat the titration to get at least two concordant readings.
Result:
1. The amount of aniline present in the whole of the given solution = g.
2. % of purity of aniline =
Calculation:
Preparation of standard potassium dichromate solution
Mass of weighing bottle + K2Cr2O7 = g
Mass of empty weighing bottle (after transferring) = g
Mass of K2Cr2O7 = g
Strength of K2Cr2O7 (in 250 ml) = M
Table: 1
Standard K2Cr2O7 solution vs. Sodium thiosulphate solution
S. No. Volume of Burette Readings (ml) Volume of Indicator

K2Cr2O7 solution Initial Final sodium
(ml) thiosulphate (ml)
1.
2.
Strength of K2Cr2O7 = M
Volume of K2Cr2O7 solution = ml.
Volume of sodium thiosulphate = ml.
Strength of sodium thiosulphate = M

Table: 2
Brominating solution vs. Sodium thiosulphate solution (Blank Titration)
S. No. Volume of Burette Readings (ml) Volume of Indicator

brominating Initial Final sodium
solution (ml) thiosulphate (ml)
1.
2.
Volume of sodium thiosulphate (A) = ml.
Table: 3
Sodium thiosulphate solution vs. Given aniline solution
S. No. Volume of given Burette Readings (ml) Volume of Indicator

solution (ml) Initial Final sodium
thiosulphate (ml)
1.
2.
Strength of sodium thiosulphate = M
Volume of given solution = ml.
Volume of sodium thiosulphate (B) = ml.
Therefore, A – B (C) = ml
The weight of aniline can be calculated by the formula given below,
C × Normality of Thio × Eq .Wt . of aniline

weight of aniline ∈100 ml=
20 ×10
The weight of aniline = g.

The percentage of aniline can be calculated by the formula given below,
0.003138× ( A−B ) × N ×100

% of Aniline=
w ×0.2
Where,
A = ml of thiosulphate required for blank.
B = ml of thiosulphate required for sample.
N = Normality of thiosulphate used.
W = weight in grams of aniline.
(0.2 N brominating solution is equivalent to 0.003138 g of aniline)
Note:
Sodium thiosulphate solution 0.1 M: It is prepared by dissolving 1.19 g KBr (M.W =
119.002 g/mol) in 100 ml distilled water and

It is prepared by dissolving 2.48 g of sodium
make up the volume in a volumetric flask.
thiosulphate pentahydrate (M.W = 248.18
g/mol) in 100 ml distilled water in a Potassium dichromate 0.016 M:
volumetric flask.
It is prepared by dissolving 1.2260 g K2Cr2O7
Starch indicator solution: (M.W = 294.19 g/mol) in 250 ml distilled water
in a volumetric flask.
Make a paste of 1 g of starch with a little water
and pour the suspension, with constant Brominating solution (0.2 M)
stirring into 100 ml of boiling water.

Weigh 1.4 g KBrO3 (M.W = 167 g/mol) and 9 g
Potassium bromate (KBrO3) 0.1 M: KBr (M.W = 119.002 g/mol) in distilled water
and make up the volume to 250 ml in a

It is prepared by dissolving 1.67 g KBrO 3 (M.W
volumetric flask.
= 167 g/mol) in 100 ml distilled water and
make up the volume in a volumetric flask. Sulphuric acid (1 M):
Potassium bromide (KBr) 0.1 M: It is prepared by dissolving 14 ml of sulphuric
acid in 250 ml of distilled water.

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2.

Estimation of Aniline by Bromination Method

To estimate the amount of aniline present in whole of the given solution by

estimated by bromination method. The method involves the following steps,

(a) Bromination of aniline by bromination mixture:

treating a mixture of potassium bromide and potassium bromate with dilute

hydrochloric acid. The bromine so liberated reacts with aniline to produce

tribromoaniline while excess of bromine remains unreacted.

5 KBr + KBrO3 + 6 HCl 3 Br2 + 3 H2O + 6 KCl

(b) Determination of unreacted bromine:

thus liberated is determined iodometrically with sodium thiosulphate solution using

2 Na2S2O3 + I2 2 NaI + Na2S4O6

Preparation of standard potassium dichromate solution

The standard potassium dichromate solution can be prepared by weighing

accurately about 1.2260 g (0.016 M) of potassium dichromate, dissolving in water and

making up to 250 ml in a standard measuring flask.

Standardization of sodium thiosulphate solution

Into a 250 ml iodine flask, pipette 20 ml of standard potassium dichromate

solution. Add 10 ml of 1 M sulphuric acid and 1 g of sodium hydrogen carbonate into

Pipette out 20 ml of brominating solution in a 250 ml iodine flask and 5 ml of

of starch-iodine complex disappears. Note the reading of thiosulphate solution required

(B). Repeat the titration to get at least two concordant readings.

1. The amount of aniline present in the whole of the given solution = g.

Preparation of standard potassium dichromate solution

Mass of weighing bottle + K2Cr2O7 = g

Mass of empty weighing bottle (after transferring) = g

Strength of K2Cr2O7 (in 250 ml) = M

Standard K2Cr2O7 solution vs. Sodium thiosulphate solution

S. No. Volume of Burette Readings (ml) Volume of Indicator

Volume of K2Cr2O7 solution = ml.

Volume of sodium thiosulphate = ml.

Strength of sodium thiosulphate = M

Brominating solution vs. Sodium thiosulphate solution (Blank Titration)

S. No. Volume of Burette Readings (ml) Volume of Indicator

Volume of sodium thiosulphate (A) = ml.

Sodium thiosulphate solution vs. Given aniline solution

S. No. Volume of given Burette Readings (ml) Volume of Indicator

Strength of sodium thiosulphate = M

Volume of given solution = ml.

Volume of sodium thiosulphate (B) = ml.

The weight of aniline can be calculated by the formula given below,

C × Normality of Thio × Eq .Wt . of aniline

The weight of aniline = g.

0.003138× ( A−B ) × N ×100

A = ml of thiosulphate required for blank.

B = ml of thiosulphate required for sample.

N = Normality of thiosulphate used.

W = weight in grams of aniline.

(0.2 N brominating solution is equivalent to 0.003138 g of aniline)

Sodium thiosulphate solution 0.1 M: It is prepared by dissolving 1.19 g KBr (M.W =

119.002 g/mol) in 100 ml distilled water and

g/mol) in 100 ml distilled water in a Potassium dichromate 0.016 M:

Starch indicator solution: (M.W = 294.19 g/mol) in 250 ml distilled water

and pour the suspension, with constant Brominating solution (0.2 M)

stirring into 100 ml of boiling water.

and make up the volume to 250 ml in a

make up the volume in a volumetric flask. Sulphuric acid (1 M):

Potassium bromide (KBr) 0.1 M: It is prepared by dissolving 14 ml of sulphuric

acid in 250 ml of distilled water.

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