Expt No.

1
Expt No 2
Expt No. 3
Use it only one this tabular column for adsorption experiment
Expt No 4
 RHS

Expt No. 5

PHASE DIAGRAM, TWO COMPONENTS WITH SIMPLE EUTECTIC AND

COMPOUND FORMATION

EXPT. NO. DATE :

AIM : To study the phase diagram for a binary mixture and to find the eutectic
temperature and the corresponding composition.

PRINCIPLE

The simplest phase diagram for a two component solid system represents
the behavior of two components which are completely soluble in each other
when in the liquid state but crystallize out in the pure state on cooling.

Substance A and substance B form a two component system of the simple,

eutectic type. Mixtures of the two substances of varying compositions are taken
and the freezing point of each melted solid solution is determined. The freezing
points of a series of liquid mixtures of varying compositions from one pure
component to the other are determined and plotted against the corresponding
composition of the liquid when two curves are obtained which will meet at a
minimum point. This is the lowest temperature at which any liquid mixture of
the two components will freeze and hence is called eutectic point.

Materials required:

(i) Substance A (pure)

(ii) Substance B (pure)

(iii) Flat bottomed tubes

(iv) Sensitive thermometer

(v) Beaker 5oml

PROCEDURE

The flat bottomed test tube with a sensitive thermometer, stirrer and
weighed amount (5g) of Substance A was mounted in the water bath. The water
bath was gradually heated while stirring. The heating was stopped when the

1
 RHS

solid melted completely to form a clear liquid. The tube was taken out from the
bath, introduced into an air jacket and allowed to cool steadily while stirring. The
freezing point was found out from the appearance of the first crystal while steady
cooling. Now a small weighed amount (0.5g) of Substance B was added to the
Substance A in the flat bottomed test tube and the freezing point of this mixture
was found out as before, as the temperature at which the first solvent crystal
separated while cooling. Similarly weighed amounts of Substance B each time
about 0.5g were added one after the other for about ten times and the freezing
point of each of the mixture was determined as before. A graph was drawn by
taking percentage composition along the X-axis & temperature along the Y- axis.

The same procedure was repeated by starting with 5g of Substance B

adding to it 10 times 0.5g portions of Substance A and finding out the freezing
points of pure Substance B and the ten resulting mixtures as before.

RESULT

The eutectic temperature =

The eutectic composition =

LHS

2
 LHS

Weight of A Weight of B Freezing

Sl.No Percentage Percentage Point OC

g g
Of A Of B

Weight of B Weight of A Freezing

Sl.No Percentage Percentage Point OC

g g
Of B Of A

%A= WA x100
WA+WB

%B= WB x100
WA+WB

3
Expt No. 6 a RHS
 RHS

LHS
 RHS

LHS

write heading
alone
LHS
Expt No. 6b
RHS
LHS
Expt No7
LHS
 RHS
Expt No. 7

DETERMINATION OF TRANSITION TEMPERATURE OF A HYDRATED SALT -

THERMOMETRIC METHOD
Aim
To determine the transition temperature of high rated salt by thermometric method
Principle
The crystalline solids on heating lose their water of crystallisation at a particular
temperature to change into an anhydrous form I.e. another form. This transition takes place at
constant temperature and accompanied by absorption or evolution of heat. The temperature at
which such a transition takes place is called a transition temperature.
The thermometric method depends on the factor temperature rises normally until the
hydrate begins to change from one form to another form. Then at a particular point the
temperature remains practically constant until transformation is complete. On cooling, the
temperature will fall at a definite rate until transition point is reached. At transition point
once again the temperature will remain practically constant for some time. The transition
temperature can be determined by plotting time on the x-axis and temperature on the y-axis.
Materials Required
1. A hydrated salt - Na2S2O3.5H2O, SrCl2.6 H2O, NaBr.3 H2O, CH3COONa.3 H2O,
MnCl2.6 H2O.
2. Transmission temperature apparatus
3. stirrer
4. Sensitive thermometer (1/10O)
5. stopwatch
Procedure
The given hydrated salt along with a few ml of a non-polar solvent such as paraffin
liquid is placed in the inner tube of the transition temperature apparatus fitted with a stirrer
and thermometer. The bulb of thermometer should be kept immersed in the sample. The
inner tube is then place the inside the outer jacket and arrangement is immersed into water
both. The temperature of the path is slowly raised by using a small flame the rate of increase
in temperature of the salt is kept uniform by slow and regular stirring. The temperature is
recorded for every minute. The temperature increases gradually and will remains constant
for some more time and again increases.
The transition temperature apparatus is taken out of the water bath. It is allowed to
cool slowly with constant stirring. The temperature is recorder for every minute. At one point
the temperature will remain constant. Cooling is continued further for some more time.
 LHS

Time TEMPERATURE
(min)
Heating (oC) Cooling (oC)

30 s
1 min
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
 RHS

A graph is plotted taking time in the abscissa and temperature in the ordinate. Two curves
will be obtained. One for heating and the other for cooling. The curve has an approximately
horizontal portion. The temperature corresponding to the horizontal portion in the graph is
noted. This gives the transition temperature of the given salt hydrate.

Report: The transition temperature of the given salt hydrate = ___________

 RHS
Expt No. 8
IODINATION OF ACETONE
AIM:
To study the kinetics of the acid catalysed reaction between acetone and iodine.
PRINCIPLE:
Acetone reacts with Iodine in the presence of an acid as a catalyst represented by the
following equation,
H+
CH3COCH3 +I2 CH3COCH2I + HI

Iodination of acetone reaction is catalysed by H+ ion. The rate of reaction is found to be

independent of the concentration of iodine.(i.e) it is zero order reaction with respect to iodine.
However it depends on the concentration of acetone and the acid catalyst. The probable
mechanism of the reaction involves two steps. In the initial step, acetone accepts a proton
from the acid HA.
fast
CH3COCH3 + HA (CH3)2C=OH+ + A-
The ion obtained changes into enol form giving up the proton to the base.
slow
(CH3)2C=OH+ + B (CH2=C(OH)CH3 + BH+
The rate reaction can be expressed as,
Rate = -d[I2]/dt = K [Acetone]l [I2]m [H+]n
in the presence of excess of acetone and acid the rate of consumption of I2, -d[I2]/dt is
independent of both concentration of acetone and acid, and the order of the reaction can be
evaluated with respect to iodine .That is
-d[I2]/dt = k1[I2]m
where k1 = K [Acetone]l [H+]n.
The progress of the reaction can conveniently be followed by tirating the samples of reaction
mixture against standard sodium thiosulphate solution and hence measuring the concentraion
of residual I2 from time to time.
REQUIREMENTS:
Thermostat at 25o C, 250cm3 conical flasks,acetone,0.5M H2SO4,0.1M I2 in 10% KI
solution,1M CH3COONa solution, standard 0.01M Na2S2O3 solution.
Procedure:
In a conical flask place 10cm3 acetone, 20 cm3 of 0.5M H2SO4 and 60cm3 of distilled
water and thermostat the flask at 25oC. Suspend 50 cm3 of I2 solution in a separate flask in the
thermostat. After the solutions have attained the equilibrium temperature, pipette 10cm3 of I2
 RHS

solution into the acetone flask. Start the stopclock when the pipette is half discharged. Mix well
the contents of the reaction mixture. Withdraw 10cm3 samples of the reaction mixture every 3
minutes and run into about 10cm3 of 1M sodium acetate and titrate it with 0.01M Na2S2O3
solution using starch solution as the indicator. The titre value gives the amount of residual
iodine in the sample.
Repeat the experiment with varying amount amounts of acetone, iodine and acid as
given in the Table below to investigate the effects of the changes in their concentrations.
LHS BOTTLE NO 1 2 3 4
Acetone 10ml 5ml 10ml 10ml
0.1M Iodine solution 10ml 10ml 10ml 5ml
0.5M H2SO4 20ml 20ml 10ml 20ml
water 60ml 65ml 70ml 60ml

CALCULATIONS:
Plot the graph of time t (abscissa) against the titre readings of Na2S2O3 solution
(equivalent to residual Iodine) for each mixture, and from the straight line so obtained deduce k
(slope= k) in each case. The straight line graph shows the reaction to be of zero order with
respect to Iodine.
From the value of rate constants for first and second sets, evaluate the order with
respect to acetone as follows.
When acetone and acid are in excess
-d[I2]/dt=k1[I2]m
k1 =[Acetone]l [Acid]n-------(1)
when acetone concentration is halved, the new value of k1’ is given by
k1’ = K [Acetone]2l [Acid]n--------(2)
From (1) and (2)
k1/ k1’ = [Acetone]l / [Acetone]2l = (2)l
Hence ,evaluate the value of l similarly from the k values for first and third sets, evaluate the
value of n, the order with respect to the acid used as the catalyst.
 LHS
Table
Bottle 1 Bottle 2

Time(mins) Volume of Na2S2O3 Time(mins) Volume of Na2S2O3

3 3
6 6
9 9
12 12
15 15
18 18

Bottle 3 Bottle 4

Time(mins) Volume of Na2S2O3 Time(mins) Volume of Na2S2O3

3 3
6 6
9 9
12 12
15 15
18 18

Calculations
k1/ k1’ = [Acetone]l / [Acetone]2l = (2)l

RHS

RESULT:
Order of the reaction between acetone and iodine with respect to acetone =
Order of the reaction between acetone and iodine with respect to acid =
Order of the reaction between acetone and iodine with respect to iodine =
Expt No. 6 RHS
ESTER HYDROLYSIS
AIM:
To determine the rate constant of acid catalysed hydrolysis of an ester and also determine
the relative strength of two acids.

PRINCIPLE:

Ethyl acetate is hydrolysed to give ethyl alcohol and acetic acid as shown below:
CH3COOC2H5 + H2O [H+] CH3COOH + C2H5OH

The reaction is catalysed by hydrogen ions. In a dilute aqueous solution of the ester,
concentration of water, being in excess, is very high and partially remain constant during the
reaction. Cconcentration of H+ which catalyses the reaction also remains constant. Thus, the
rate of reaction is dependent only on the concentration of the ester,
dx/dt = k [CH3COOC2H5]
Following the kinetic equation of first order

k = 2.303 log (a/a-x)

t
Since acetic acid is produced as a result of hydrolysis, the kinetic of the equation can be
followed by withdrawing a fixed volume of the reaction mixture from time to time and
titrating with a standard alkali. The titre value is equivalent to the sum of the acid used as the
catalyst, which remains constant throughout, and of the acetic acid produced during the
reaction. The difference of titre values at any time after the commencement of the reaction
and that at the commencement give the acetic acid formed and hence the amount of methyl
acetate hydrolysed at that instant takes place.
Rate constants of the reaction catalysed by equal concentration of the acids are directly
proportional to the degree of dissociation of the respective acids. Thus, the relative strength
is given by:
Relative strength = strength of one acid/strength of the other acid = a1/a2 = k1/k2
Where, a1 and a2 are the degree of dissociation of the two acids, and k1 and k2 are the rate
constants in presence of the respective acids.

REQUIREMENTS:

Thermostat, 250cm3 and 150cm3 conical flask, 5cm3 pipette, Stop watch, Methyl acetate,
250cm3, 0.5M HCl, 500cm3 approx 0.5N NaOH, Phenolphthalein indicator,

PROCEDURE:

1. Take 100cm3 0.5M HCl in a dry 250cm3 conical flask and clamp it in the thermostat at
30°C. Suspend also a stopper tube in the thermostat at 30°C and place in it about 20cm3 of
ethyl acetate.
 RHS
2. Fill a burette with0.1M NaOH solution, previously rinsing it with the same solution. Take
3-4 conical flasks containing pieces of clean ice.
3. When temperature equilibrium has been reached pipette out 5cm3 of the ester into the
conical flask of acid. Shake well and immediately pipette 5 cm3 of the reaction mixture into a
conical flask containing ice cold water so as to arrest the reaction. Record the time to the
nearest 10sec when the pipette has been half discharged into the flask. Titrate this solution as
rapidly as possible with 0.5N NaOH using phenolphthalein as indicator. The titre value gives
the amount of HCl in the sample at the start of the reaction(Vo).
4. Make similar titrations of further 5cm3 samples of the reaction mixture at successive
intervals of 10, 20, 30, 40, 60, 90 and 120mins(Vt).
5. Place the reaction vessel containing the remaining reaction mixture; with its cork closed
loosely in water bath at about 50°C for at least one hour to complete the reaction. Then after
cooling the flask to room temperature titrate 5cm3 of sample as before (V∞).
6. Repeat the same experiment for the given acid 2.
7. Plot the graph of log(V∞-Vt) vs time . Calculate the rate constant from the slope of the
straight line obtained by the equation
k = - 2.303 x slope

6.Calculate the ratio of reaction rate constant in the two given acid catalysts.. This gives the
relative strength of the two acids.

CALCULATION:
LHS
The specific rate constant is calculated by the equation

k = 2.303 log (V -Vo)/V -Vt)

t

RESULT: RHS
i) By calculation
The specific rate constant for the acid catalysed hydrolysis of an ester
acid A k1 = min-1
acid B k2 = min-1
Relative strength of acid 1 and 2 k1/k2 =

ii) By graph
The specific rate constant for the acid catalysed hydrolysis of an ester
acid A k1 = min-1
acid B k2 = min-1
Relative strength of acid 1 and 2 k1/k2