Lab Manual
Lab Manual
Lab Manual
(2160506)
Student Name:-_________________________________________
Batch:-________________________________________________
Certificate
This is to certify that, Mr. /Ms. _______________________________
Enroll. No. _______________________ of sixth semester Bachelor of
Chemical Engineering has completed the term work satisfactorily in
Chemical Reaction Engineering I (2160506) for academic year as
prescribed in the GTU curriculum.
Place:-__________ Date:-_____________
EXPERIMENT NO. 1
Aim: -To determine the activation energy of the reaction between sodium thio-sulphate
and HCl using Arhenious Equation.
Apparatus: -
Glass beaker
Thermometer
Stop watch
100 ml measuring Cylinder
Paper
Chemicals: -
0.3 N sodium thiosulphate
0.3 N HCl solution
Theory:-
For many reaction and particularly elementary reactions, the rate expression can be written as
a product of temperature dependent term & a composition dependent term as
Y = F1 (Temperature) x F2 (Composition)
= K x F2 (Composition)
For such reaction the temperature dependent term, the reaction rate constant was found in
particularly all cases to be well represented by Arhenius law :
K = K0 e (-E/RT)
Where K is called the frequency factor and E is the activation energy of the reaction. Thus
expression fits experimental data well over the temperature ranges and it strongly suggest
from various points as being a very good approximation to the true temperature dependency.
The temperature dependency of the reaction is determined by the activation energy and
temperature. Level as shown by curve of ln K Vs 1/T.
1. From Arhenious law, plot of lnK Vs 1/T gives a straight line with large slope for a
large E and small slope for small E.
2. Reaction with high activation energy is very temperature sensitive, reaction with low
activation energies are relatively temperature sensitive.
3. For the Arhenious law, the frequency factor K0 does not affect the temperature
sensitivity of a reaction.
Procedure :-
1. About 20 ml of each reactant has been taken in to two separate glass beacker.
2. Both solutions were heated until they reached a steady state value of temperature,
which is noted in the observation table.
3. The beaker containing sodium thiosulphate on a paper on which a cross mark was
made.
4. The HCl solution was then poured in the other beaker and then the beaker was stirred
simultaneously the stop watch was started.
5. The cross sign ceased to be invisible due to formation of sulphur ppts. was noted in
the observation table.
6. Similarly the complete procedure was repeated for a different steady state temperature
and a graph of ln t Vs 1/T was plotted.
Reaction: -
EXPERIMENT NO. 2
Aim: -To determine order of reaction for the reaction between sodium thiosulphate and
HCl.
Apparatus: -
250 ML Glass beaker
Thermometer
Stop watch
100 ml measuring Cylinder
Paper
Chemicals: -
0.1, 0.2, 0.3, 0.4 N sodium thiosulphate
0.1, 0.2, 0.3, 0.4 N HCl solution
Theory:- Some time for the irreversible reaction A + B + … → Product. We may write,
-rA = dCA / dt = k CAa CBb
If the reaction are present in their stoichiometric ratios, they will remain at that ratio through
the reaction. Thus for reactant A and B at any time CA/C B and we may write integration for
n=1 gives.
The full time method requires making a series of run, each at a different initial concentration
and shown that the fractional conversion in a given time rises with increased concentration
for orders grater than one drops with increased concentration for reaction first order.
Defining the full time for the reaction to complete as the time needed for the concentration of
reactants to drop to zero we obtain. This expression shows that a plot of ln tl Vs. ln CA0
1-n
CA0
t= (1-n) x k
Procedure :
1. Prepare solution of sodium thio sulphate of 0.1, 0.2, 0.3, 0.4 N.
2. Also prepare solution of HCl of above concentration.
3. Now take 20 ml of 0.1 N sodium thiosulphate in a beaker and put it over a white
paper, which is cross-marked.
4. Now, 20 ml of 0.1 N HCl solution is then poured in the same beaker and the mixture
was stirred simultaneously and the stopwatch is also started.
5. The cross sign is watched through the reaction mixture and the time when the cross
sign doesn’t see due to formation of sulfur precipitate is noted.
6. Similarly follow the same procedure for the other concentration of sodium
thiosulphate and HCl.
EXPERIMENT NO. 3
Aim: -To measure the kinetics of a reaction between ethyl acetate and sodium hydroxide
under condition of excess ethyl acetate at room temperature.
Apparatus: -
500 ml Glass beaker
Pipette
Burette
Thermometer
Stop watch
100 ml Conical flask
Chemicals: -
Ethyl acetate
NaOH
Std. HCl
Theory:-
Under normal conditions, reactions between ethyl acetate and NaOH is of second order. How
ever if concentration of one of the reactants is in excess it remains constant through the
reaction. Hence the above reaction is a pseudo first ofder reaction and a apparently a first
order reaction. This fact is verified by this experiment.
Procedure:-
1. Take 150 ml of ethyl acetate in a beaker, which serve as a batch reactor.
2. Add 150 ml of 0.1 N NaOH to ethyl acetate.
3. stir the content of the beaker while simultaneously starting the stopwatch.
4. Take 6 samples of 10 ml each from the beaker at an interval of three min.
5. Content of the flask are titrated against 0.1 N HCl.
6. From the titration values it is possible to determine concentration of NaOH.
7. Temperature of the reaction is noted.
EXPERIMENT NO. 4
Aim: -To determine the kinetics of the reaction between ethyl acetate and sodium hydroxide
at room temperature by the integral method of analysis.
Apparatus: -
500 ml beaker
Stop watch
100 ml conical flask
Thermometer
Pipette
Burette
Chemicals: -
Ethyl acetate
NaOH
Std. HCl
Theory:-
In the integral method of analysis, the order of reaction under consideration assumed and the
integral rate expression is subsequently obtained on based on this suitable graph is drawn by
using the experimental data which reveals the fitness of such data. If the fit is satisfactory
then the assumed order is correct, otherwise a different order is assumed and the same
method is continued until a satisfactory it is obtained. It is also possible to calculate fro the
graph the rate constant, thus the kinetics of a specified temp can be determined.
Procedure:-
1. 150 ml of ethyl acetate of 0.3 N is taken in the 50 ml beaker, which serves as the
batch reactor.
2. To this 150 ml of NaOH solution of 0.2 N is added and the contents are kept well
stirred.
3. Soon after adding NaOH a stopwatch is started.
4. In all samples each of 10 ml volume are taken from the reactant contents as per the
following time schedule.
Observations: -
Room temperature : ________
0.3 N ethyl acetate – B
0.2 N NaOH – A
0.2 N HCl in burette and indicator phenolphthalein
EXPERIMENT NO. 5
Aim: -To determine the activation energy and frequency factor for reaction between ethyl
acetate and sodium hydroxide at room temperature & at different temperature.
Apparatus: -
500 ml Glass beaker
Storage tanks 1000 ml
Conical flask
Stop watch
Pipette
Burette
Thermometer
Chemicals: -
Ethyl acetate
NaOH
Std. HCl
Distilled water
Procedure:-
1. Initially the experiments carried out at room temperature. Six conical flask are kept in
order, in each one of them same amount of water is added.
2. 100 ml of ethyl acetate (0.3 N) is taken in order in each one of them in 500ml beaker,
which serves as the batch reactor.
3. To this, 100 ml of NaOH (0.2 N) is added and content are kept well stirred.
4. A stopwatch is started simultaneously for every 3 min. 10 ml of sample is pipetted out
from the reactor and transferred to the conical flask which already contains water.
5. The presence of water reduces the concentration of reactant thereby decreasing the
rate of reaction.
6. The contents of the conical flask are immediately titrated against 0.1 N HCl from the
titration value, the concentration of NaOH is found out.
7. Temperature of reaction is noted.
EXPERIMENT NO. 6
Aim: -To determine the kinetics of the reaction between ethyl acetate and sodium hydroxide
at room temperature by the differential method of analysis.
Apparatus: -
500 ml Glass beaker
150 ml Conical flask
Stop watch
Pipette
Burette
Thermometer
Chemicals: -
Ethyl acetate
NaOH
Std. HCl
Distilled water
Theory:-
The differential method of analysis given straight way. The kinetics of the reaction unlike
integral method where trial and error technique is involved. In case of constant volume
reactor, as in the present case the time derivative of concentration gives the rate of reaction.
This is easily obtained from the concentration history of reactant or product.
At any time, the rate of depletion of NaOH is given by
Where,
from stochiometry we have CA = CB. This is because of equal initial conc. Of reactants.
Hence,
p = another constant
A plot of ln (-dCA / dt) Vs CA yields a straight line. The slope is p which gives the
Procedure:-
1. 150 ml ethyl acetate of 0.15 N is taken in 500 ml beaker which serves as a batch
reactor.
2. To this, 150 ml of NaOH solution (0.15 N) is added & then contents are kept well
stirred.
3. A stopwatch is started simultaneously. In given time interval, 10 ml of the sample is
taken.
Reaction: -
CH3COOC2H5 + NaOH → C2H5OH + CH3COONa
(B) (A)
EXPERIMENT NO. 7
Aim: -To determine the kinetics of the reaction between n- butyl acetate and sodium
hydroxide at room temperature by the integral method of analysis.
Apparatus: -
500 ml Glass beaker
100 ml Conical flask
Stop watch
Pipette
Burette
Thermometer
Chemicals: -
Butyl acetate
NaOH
Std. HCl
Theory:-
In the integral method of analysis, the order of reaction under consideration Is assumed and
the integral rate expression if subsequently obtained. Based on this, a suitable graph is drawn
using the experiments data which reveals the fitness of such data. If the fit is correct
otherwise a different order is assumed & the same method is continued until the satisfactory
fit is obtained. It is also possible to calculate from the kinetics at a specified temperature can
be determined.
Procedure:-
1. 150 ml butyl acetate of 0.1 N is taken in 500 ml beaker which serves as a batch
reactor.
2. To this, 150 ml of NaOH solution (0.09 N) is added & then contents are kept well
stirred.
3. Soon after adding NaOH, start stopwatch.
4. In all 12 samples each of 10 ml volume are taken from the reactor content as per the
following time schedule.
1, 2, 3 → for every 2 min
4, 5, 6 → for every 3 min
7, 8, 9 → for every 5 min
10, 11→ for every 10 min
5. In each case, the volume of sample pipetted is immediately transferred to conical
flask containing 25 ml of water which reduces the conc of NaOH thereby thoroughly
decreasing the rate of reaction.
6. The contents of the conical flask are titrated against 0.1 N HCl & the con of NaOH is
obtained. The temperature of the reaction is noted.
Reaction: -
CH3COOC4H5 + NaOH → C4H5OH + CH3COONa
(B) (A)
EXPERIMENT NO. 8
Aim: -To determine the kinetics of the reaction between n- butyl acetate and sodium
hydroxide at room temperature by the differential method of analysis.
Apparatus: -
500 ml Glass beaker
100 ml Conical flask
Stop watch
Pipette
Burette
Thermometer
Chemicals: -
Butyl acetate
NaOH
Std. HCl
Theory:-
The differential method of analysis given straight way. The kinetics of the reaction unlike
integral method where trial and error technique is involved. In case of constant volume
reactor, as in the present case the time derivative of concentration gives the rate of reaction.
This is easily obtained from the concentration history of reactant or product.
Where,
K = rate constant
M, n = order of reaction with respect to A & B
The above equation is valid for constant volume system as is usual with liquid phase
reaction from stochiometry we have CA = CB. This is because of equal initial conc. of
reactants. Hence,
p = another constant
A plot of ln (-dCA / dt) Vs CA yields a straight line. The slope is p which gives the
Procedure:-
1. 150 ml butyl acetate of 0.15 N is taken in 500 ml beaker which serves as a batch
reactor.
2. To this, 150 ml of NaOH solution (0.15 N) is added & then contents are kept well
stirred.
3. Soon after adding NaOH, start stopwatch.
4. In all 12 samples each of 10 ml volume are taken from the reactor content as per the
following time schedule.
1, 2, 3 → for every 3 min
4, 5, 6 → for every 5 min
7, 8, 9 → for every 10 min
5. Transfer each sample to a conical flask containing 25 ml of water.
6. The presence of water reduces the concentration of reactants, thereby lowering the
rate of reaction.
7. Titrate the contents of the conical flask against 0.1 N HCl immediately.
8. The conc. Of NaOH unreacted is found from the titration reading.
9. Plot con. Vs time data graph for NaOH and Observe the temperature of the reaction.
Reaction: -
CH3COOC4H9 + NaOH → C2H9OH + CH3COONa
(B) (A)