Jawaharlal Nehru Engineering College

Laboratory Manual

CHEMICAL REACTION ENGINEERING

For

Third Year Students Chemical Engineering

16, Dec 2003 Rev 00 Chem Engg. ISO 9000 Tech Document

Author JNEC, Aurangabad

 FORWARD

It is my great pleasure to present this laboratory manual for Final year engineering
students for the subject of Chemical Reaction Engineering keeping in view the vast
coverage required for visualization of concepts of Industrial Pollution Control with
simple language.

As a student, many of you may be wondering with some of the questions in your
mind regarding the subject and exactly what has been tried is to answer through
this manual.

As you may be aware that MGM has already been awarded with ISO 9000
certification and it is our endure to technically equip our students taking the
advantage of the procedural aspects of ISO 9000 Certification.

Faculty members are also advised that covering these aspects in initial stage itself,
will greatly relived them in future as much of the load will be taken care by the
enthusiasm energies of the students once they are conceptually clear.

Principal
 LABORATORY MANNUAL CONTENTS

This manual is intended for the Third year students of Chemical Engineering
branch in the subject of Chemical Reaction Engineering. This manual typically
contains practical/Lab Sessions related Reaction Engineering covering various
aspects related to the subject to enhance understanding.

We have made the efforts to cover various aspects of the subject Chemical Reaction
Engineering in chemical industry to make it meaningful, elaborative
understandable concepts and conceptual visualization.

Students are advised to go thoroughly through this manual rather than only topics
mentioned in the syllabus as practical aspects are the key to understanding and
conceptual visualization of theoretical aspects covered in the books.

Good Luck for your Enjoyable Laboratory Sessions

SUBJECT INDEX

1. Interpretation of batch reactor data.

2. To study the kinetics of liquid phase irreversible reaction in a batch reactor.

3. To study the kinetics of liquid phase reversible reaction in batch reactor.

4. Conversation in CSTR.

5. Conversation in PFR.

6. Saponification of Ethyl Acetate

7. To determine the pseudo first order rate constant. (TBC)

8. To study the kinetics of liquid phase reaction by dilatometer method.

DOs and DONT DOs in Laboratory:

1. Do not enter the laboratory without wearing apron, preferably use shoes.

2. Safety should be given topmost priority.

3. Follow the instructions given by the teacher.

4. Do not touch any Equipment/Chemicals without prior permission.

5. Check the glassware before getting issued.

6. Handle the chemicals carefully as per instructions.

7. Do not pipette any solution/chemical with mouth.

8. During performance of the practical if any glassware is broken inform immediately.

9. Return the borrowed apparatus after the expt is over.

10. Observe safety precautions while performing the expts.

Instruction for Laboratory Teachers::

1. Submission related to lab work completed, should be done before the next lab session.

2. The promptness of submission should be encouraged by way of marking and evaluation patterns
that will benefit the sincere students.

WARMUP EXCERCISES:

Define Reaction Rate, Rate constant, Activation Energy, Space Time, Space Velocity,
Molecularity, Order Of Reaction, Equation Representing Batch Reactor, CSTR, PFR
Different Types of Industrial Reactors,
Different Application of Chemical Reaction Engineering.
 Exercise No1: ( 2 Hours)
Interpretation of Batch Reactor data

A] Aim: To study the interpretation of Batch Reactor Data.

Theory: --
1) Integral Method of Analysis:

2) Differential Method of Analysis: ---

Conclusion--
Exercise No2: ( 2 Hours)
Batch Reactor for irreversible reaction.

A] Aim: To study batch reactor kinetics for ethyl acetate - NaOH and find the value of rate constant.

Procedure:
1) Take the solution of NaOH (0.1N) and ethyl acetate (0.1N) of desired concentration
inside the batch reactor.
2) The mixture in the reactor is continuously stirred and the stirred is maintained at
constant speed
3) Take out sample in a beaker from reactor at constant time difference.
4) Add 20ml of 0.1N HCL in the sample.
5) Titrate the sample against 0.1N NaOH using phenolphthalein as an indicator.
6) Repeat the above procedure six times.

Observations:

1) Normality of NaOH solution (N3) = 0.1N

2) Normality of Ethyl acetate solution = 0.1N
3) Normality of HCL solution (N1)= 0.1 N
4) Volume of HCL solution (V1)= 20 ml
5) Volume of NaOH (V3) in burette
6) Volume of sample (V2) = 10 ml

Observation Table:

Sr.No. Time Vol.of Normality XA -Ln (1-XA)

(Sec.) NaOH (ml) CA = N2
1
2
3
4
5

Calculations:
CA= N2 =N1V1-N3V3 / V2

From graph of -Ln (1-XA) Vs Time

Calculate the slope K (Sec -1)

Result:
Exercise No3: ( 2 Hours)
Batch Reactor for rreversible reaction.
A] Aim: To study batch reactor kinetics for Acetic acid - Methanol and find the value of rate constant.

Procedure:
1) Take the solution of Acetic acid (0.1 N) - Methanol (0.1 N) of desired concentration
inside the batch reactor.
2) The mixture in the reactor is continuously stirred and the stirred is maintained at
constant speed
3) Take out sample in a beaker from reactor at constant time difference.
4) Titrate the sample against 0.1N NaOH using phenolphthalein as an indicator.
5) Repeat the above procedure six times.

Observations:

1) Normality of NaOH solution (N1) = 0.1N

2) Normality of Acetic acid solution = 0.1N
3) Normality of Methanol solution = 0.1 N
4) Volume of NaOH (V1) in burette
5) Volume of sample (V2) = 10 ml

Observation Table:

Sr.No. Time Vol.of Normality XA -Ln (1-XA)

(Sec.) NaOH (ml) CA = N2
1
2
3
4
5

Calculations:
CA= N2 =N1V1 / V2
CA = CA0-CA/CA0

From graph of -Ln (1-XA) Vs Time

Calculate the slope K (Sec -1)

Result:
Exercise No4: ( 2 Hours)
Continuous stirred tank reactor

A] Aim: To carry out saponification of ethyl acetate in given CSTR and to determine the conversion and to compare with the
theoretical

Procedure:
1) Standardized solution of 0.1 N ethyl acetate, 0.1 N NaOH and 0.1 N HCL are used.
2) The observed tanks are filled with NaOH and ethyl acetate solution.
3) The mixture in the reactor is continuously stirred and the speed of the stirrer is maintained at
constant value.
4) Determine the residence time in the reactor by starting the flow of NaOH solution and
measuring the flow rate with rotameter (Vol of reactor/Volumetric flow rate = m3/sec or
liters/LPM)
5) Start the flow of ethyl acetate and check that its flow rate is also the same as of NaOH and
such that ample time is allowed for the reaction to reach steady state (Approximately 10
times the residence time))
6) Take 20 ml of 0.1 N HCL in a flask and add 10 ml of reaction mixture (from outlets) to the flask.
7) Back titrate the mixture in the flask with 0.1 N NaOH using phenolphthalein as an
indicator
8) Take five more samples from reacting streams

Observations:
1) Standardization NaOH solution
2) Standardization HCL solution
3) Normality of NaOH solution = ________N
4) Normality of HCL solution =_______N1
5) Normality of NaOH solution used for back titration = _________N3
6) Reactor Volume = ______V
7) Volume of sample collected =_________V2
8) Volume of HCL taken = _________V1
9) Volume of NaOH rundown in back titration = _________V3
10) Concentration of A (i.e. Ethyl Acetate) can be calculated as
CA = N1V1 N3V3 / V2

Observation Table:

Sr.No. Flow Rate of Flow Rate of Sample NaOH Time

ethyl acetate NaOH Collected V3 (ml) (Sec.)
(LPM) (LPM) V2 (ml)
1
2
3
4
5

Calculations:
F = FA+FB/2

Initial concentration of A = CA0 = FA *N (EA) / FA+FB

N (EA) =Normality of ethyl acetate
CB = (CB0-CA0) +CA
Where CB0 = FB *N (NaOH) / FA+FB

And
Reaction rate rA =F (CA0-CA)/V
XA = CA0-CA/CA0
Prepare a table as follows:
Sr.No. CA0 CB0 CA CB XA
1
2
3
4
5

Result:
1) Report the values of residence times in the reactor.
2) Report the values of average conversion for saponification of ethyl acetate
Exercise No5: ( 2 Hours) 1 Practical
Plug Flow Reactor
A] Aim: To carry out saponification of ethyl acetate in given PFR and to determine the conversion experimentally

Procedure:
1) Start the flow rate to achieve steady-state condition. (Flow rate of NaOH)
2) Then start the flow rate of ethyl acetate and ensure NaOH as well as ethyl acetate flow rate
are at steady state.
3) Take 20 ml sample of mixture and add 20 ml of 0.1 N HCL and then titrate with NaOH (0.1 N)
4) Continue taking reading until constant burette reading is obtained (at least 10 readings)
5) Find the practical conversion of PFR

Observations:
1) Normality of NaOH solution (N3)= 0.1N
2) Volume of NaOH (Burette Reading, V3) = _________
3) Normality of Ethyl acetate solution = 0.1N
4) Normality of HCL solution (N1)= 0.1 N
5) Volume of HCL solution (V1) = _______
6) Volume of sample (V2) = __________-
7) Reactor Volume = ______ml
8) Flow rate of NaOH solution = _________ LPM
9) Flow rate of Ethyl acetate solution = _________LPM

Observation Table:

Sr.No. Time Burette Reading XA

(Sec.) (ml)
1
2
3
4
5

Calculations:
Limiting reactant is ethyl acetate

N2 = N1V1 N3V3 / V2
N2 = Normality of unreacted NaOH
CA = CA0 (M-X=) = CA0 (CB0 /CA0 XA)
N2 = CA0 (CB0 /CA0 XA)
Hence calculate XA i.e. practical conversion.

Result:
Practical conversion in PFR = _____
Exercise No6: ( 2 Hours)
Saponification of Ethyl Acetate

A] Aim: To determine that the saponification of ethyl acetate in dilute aqueous solution is a second order reaction and to
report the value of the reaction rate constant.

Procedure:
1) Prepare 0.1 N NaOH solution
2) Place 400 ml of alkali solution in a clean 1 lit. Flask, which serve as a reactor. Add 25 ml
of HCL (0.1 N) solution in to each of 1,2,3.Flask
3) Place the reactor on a magnetic stirrer and start stirring vigorously. Keep a clean and
dry 25 ml pipette handy.
4) By using pipette transfer exactly 1.96 ml of ethyl acetate solution in to the reactor and
start stopwatch simultaneously. The ethyl acetate itself forms a 0.05 M solution.
in a rector itself and the saponification reaction is now on.
5) At a reaction time of 1,2,3. 12 min. pipette out 25 ml of reaction mixture into each
one of the labeled conical flask.
6) Back titrate the content of the 12 conical flasks with NaOH using phenolphthalein as
an indicator.

Observations:
1) Standardization NaOH solution
2) Standardization HCL solution
3) Standardization Ethyl acetate solution
4) Normality of NaOH solution (N3) = ________N
5) Volume of NaOH solution (V3) = _________
6) Normality of HCL solution (N1) =_____
7) Volume of HCL solution (V1)= _______
8) Volume of reaction mixture (V2)= __________

Observation Table:

Sr.No. Time Volume of CA 1/CA CA2 -dCA/dt

Sec NaOH (ml)
1
2
3
4
5

Calculations:
N2 = CA = N1V1 N3V3 / V2

Graphs: 1) CA Vs Time
2) dCA/dt Vs CA2
3) 1/CA= Vs Time

Result:
Exercise No7: ( 2 Hours)
Hydrolysis of tertiary butyl chloride

A] Aim: To determine the pseudo first order rate constant for the hydrolysis of TBC

Chemicals required:
Solution of TBC in acetone of 0.1N,NaOH solution of 0.05 N, bromophenol blue indicator,250 ml
conical flasks, measuring pipette, stop watch, distilled water, standardized oxalic acid

Procedure:
1) Pipette precisely 3ml of 0.1 N TBC into a clean and dry 25 ml conical flask (1)
2) Pipette precisely 0.6ml of 0.05 N NaOH into another clean and dry 25 ml conical flask (2) .To
this add 6.4 ml of distilled water by means of pipette (Use different pipettes for different
solutions)
3) Add a drop of bromophenol indicator into flask (No.2). This will give a deep blue indication.
Observe the color by placing it on a tile or a plain paper
4) Add contents of flask (2) to flask (1) starting the stopwatch simultaneously mix the solution
thoroughly and then pour it back to flask (2) and watch for change of color
5) When the solution color changes from deep blue to greenish yellow stop the stopwatch and
note the time.
6) Repeat the experiment with different quantities of NaOH
7) Determine the exact normality of NaOH solution before starting the experiment the
experiment. The value of the fraction of conversion XA depends on exact normality of NaOH
solution
8) Note the room temperature

Observations:
Normality of NaOH solution = ________N
Normality of TBC = _______N

Observation Table:

Sr.No. Volume of Volume of Volume of Time XA Ln [1/1-XA]

TBC (ml) NaOH (ml) water (ml) Sec
1
2
3
4
5

Calculations:
XA = NNaOH * VNaOH / NTBC * VTBC

CB0 = Concentration of H2O= ______ gmmole /lit

ln[1/1-XA] Slope = k

time (sec)

kI = k / CB0

6) Result: The pseudo first order rate constant = k=

7) The pseudo second order rate constant = kI =
7. Quiz on the subject:
Quiz should be conducted on tips in the laboratory, recent trends and subject knowledge of the subject.
The quiz questions should be formulated such that questions are normally are from the scope outside of
the books. However twisted questions and self formulated questions by the faculty can be asked but
correctness of it is necessarily to be thoroughly checked before the conduction of the quiz.

8. Conduction of Viva-Voce Examinations:

Teacher should oral exams of the students with full preparation. Normally, the objective questions with
guess are to be avoided. To make it meaningful, the questions should be such that depth of the students
in the subject is tested Oral examinations are to be conducted in co-cordial environment amongst the
teachers taking the examination. Teachers taking such examinations should not have ill thoughts about
each other and courtesies should be offered to each other in case of difference of opinion, which should
be critically suppressed in front of the students.

9. Submission:
Document Standard:
A] Page Size A4 Size
B] Running text Justified text
C] Spacing 1 Line
D] Page Layout and Margins (Dimensions in Cms)
Normal Page Horizantal

2.0

2.5

2.0
2.5 2.0 2.0

0.7
0.7
2.0

2.0
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Document Subject Century Gothic 14 ----- ------ --------- Capital
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Forward heading Bookman old Slyle 12 ----- ------ Yes Capital
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Index title Bookman old Slyle 12 Yes ------ Yes Capital
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9. Evaluation and marking system:

Basic honesty in the evaluation and marking system is absolutely essential and in the process impartial
nature of the evaluator is required in the examination system to become popular amongst the students.
It is a wrong approach or concept to award the students by way of easy marking to get cheap popularity
among the students to which they do not deserve. It is a primary responsibility of the teacher that
right students who are really putting up lot of hard work with right kind of intelligence are correctly
awarded.

The marking patterns should be justifiable to the students without any ambiguity and teacher should
see that students are faced with unjust circumstances.