Jawaharlal Nehru Engineering College

Laboratory Manual

CHEMICAL REACTION ENGINEERING

For

Final 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 MANUAL CONTENTS

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

We have made the efforts to cover various aspects of the subject Industrial
Pollution Control in chemical industry will be complete in itself to make it
meaningful, elaborative understandable concepts and conceptual
visualization.

Students are advised to thoroughly go 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) Solid Liquid System

2) Liquid Liquid system

3) RTD in Non Ideal Reactor ( CSTR)

4) RTD in Dispersion Model ( Packed Bed Reactor)

5) RTD in Plug Flow Reactor

6) Temperature Dependency of Reaction Rate

7) Conversion in CSTRS in series

8) Industrial Reactors
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 should be completed 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.
Exercise No1: ( 2 Hours) 1 Practical
Solid-Liquid Systems
A] Aim: To calculate the mass-transfer coefficient (KSL) for physical and chemical dissolution and to calculate the
enhancement factor for solid-liquid systems

Procedure:
I] Physical Dissolution
1) Initially Measure the dimensions of benzoic acid rod (length,dia,area and volume )
2) Take about 345 ml water in a beaker such that the benzoic acid rod dips completely
in the water
3) Start the stirrer and take out samples from beaker at an interval of 3 min and titrate it
against 0.02N NaOH solution
4) Repeat the above procedure six times.
5) Measure the dimensions of benzoic acid rod at the end of this set

II] Chemical Dissolution

1) Take about 345 ml, O.1N NaOH in a beaker such that the above used benzoic acid
rod dips completely in NaOH solution
2) Start the stirrer and take out samples from beaker at an interval of 3 min and titrate it
against 0.1N Oxalic acid
3) Repeat the above procedure six times.
4) Measure the dimensions of benzoic acid rod at the end of this set

Precautions
1) The benzoic acid rod should completely dip in water as well as in NaOH solution .
2) The speed of the stirrer should be less and it should be same in both the cases
3) The dimensions of benzoic acid rod should be measured before and after each set.

Graphs :
Plot a graph of Ln (CA*/CA*-CA) Vs Time for physical dissolution and find its slope
Plot a graph of CB0-CB Vs Time for chemical dissolution and find its slope

Observations:
SET-I
1) Diameter of benzoic acid rod = D1 = ___________ mm
2) Length of benzoic acid rod = L1 = _________mm
3) Diameter of shaft = d = _________ mm
4) Normality of NaOH in burette = 0.02N
5) CA* = _______ gm moles/lit (From Perrys Handbook)
6) Diameter of benzoic acid rod after 1st set = D2 = _______mm
7) Length L2 = _________mm

Observation Table:

Sr.No. Burette Time Normality Ln (CA*/CA*-CA)

reading min CA = N gm
V1 ml gmole / lit
1
2
3
4
5

Calculations:
CA= N =N2 V2 / V1

Surface Area = A1 = ( D1 L1+2 R12 ) - 2 r2 m2

Where r =d/2
Surface Area = A2 = ( D2 L2+2 R22 )-2 r2 m2
Total area A = A1+A2/2= ______m2

V = Volume of water +Volume of Benzoic acid rod m3

a = A/ V

SET-II
1) Normality of NaOH = CB0 = 0.1 N
2) Normality of Oxalic Acid in burette = 0.1N
3) Sample taken = V4 = 10 ml
4) Diameter of benzoic acid rod after 2nd set = D3 = _______mm
5) Length L3 = _________mm

Observation Table:

Sr.No. Burette Time Normality CB0-CB

reading min CB = N gm
V3 ml gmole/lit
1
2
3
4
5

Calculations:
CB= N =N2V2 / V1
Surface Area = A3 = ( D3L3+2 R32 )-2 r2 m2
Total area A = A2+A3/2= ______m2

V = Volume of NaOH +Volume of Benzoic acid rod m3

a = A/ V

Result:
Mass transfer coeffiecient for physical dissolution KSL = ____ m/min
Mass transfer coeffiecient for chemical dissolution KSL* = ____ m/min
Enhance factor = KSL* / KSL = _________

Conclusion :
Exercise No2: ( 2 Hours) 1 Practical
Liquid-Liquid Systems
A] Aim: To calculate the mass-transfer coefficient for physical and chemical dissolution and to calculate the
enhancement factor for liquid-liquid systems

Procedure:
I] Physical Dissolution
1) Measure the dimensions of the beaker
2) Take about 400 ml water in a beaker and add about 50ml butyl acetate
3) Start the stirrer and take out samples from beaker at an interval of 3 min and titrate it
against 0.05 N NaOH
4) Repeat the above procedure six times.

II] Chemical Dissolution

1) Take about 400 ml, O.14N NaOH in a beaker and add about 50ml butyl acetate
2) Start the stirrer and take out samples from beaker at an interval of 3 min and titrate it
against 0.1N Oxalic acid
3) Repeat the above procedure six times.

Observations:
SET-I
1) Diameter of beaker = D = ___________ mm
2) Diameter of shaft = d = _________ mm

3) Normality of NaOH in burette = N

4) Volume of Butyl Acetate taken = _______ml
5) Volume of sample taken = V2 = 10 ml
6) Volume of water taken = _________ ml
7) CA* = _______ gm moles/lit (From Perrys Handbook)

Observation Table:

Sr.No. Burette Time Normality Ln (CA*/CA*-CA)

reading min CA = N2
V1 ml gmole/lit
1
2
3
4
5

Calculations:
CA= N2 =N1V1 / 10

Surface Area = A = /4 (D)2 - / 4 (d)2 m2

V = Volume of water +Volume of Butyl Acetate m3
a = A/ V

From graph of Ln (CA*/CA*-CA) Vs Time

Calculate the slope = KSL * a
KSL = / a m/min
SET-II
1) Normality of NaOH = CB0 = 0.14 N
2) Normality of Oxalic Acid = N3 = ____ N
3) Sample taken = V4 = 10 ml

Observation Table:

Sr.No. Burette Time Normality CB0-CB

reading min CB = N4
V3 ml gmole/lit
1
2
3
4
5

Calculations:
CB= N4 =N3V3 / 10

From graph of V CB0-CB Vs Time

Calculate the slope = KSL* . a . CA*
KSL* = / a * CA* m/min

Enhancement Factor = E = KSL* / KSL = _______

Result:

Conclusion :
Exercise No3: ( 2 Hours) 1 Practical
Non Ideal Reactor (CSTR) -RTD
A] Aim: To study residence time distribution (RTD) in a CSTR and to find out peclet No.

Procedure:
1) Standardised solution of 0.05N oxalic acid is used for back titration .
2) Start the flow of water in the CSTR and maintain it at a constant value also start the
stirrer and keep the speed of agitation suffiecient enough for proper mixing and at a
constant value
3) Take 10 ml of 1N NaOH in a syringe and inject all of it at one instant in the reactor and
start the stopwatch simultaneously .
4) Take known volume of sample at the outlet of the reactor every ten seconds and
titrate this using 0.05N oxalic acid
5) Take at least 18 readings.

Observations:
1) Normality of NaOH = 1N
2) Flow rate of water = Fw (ml/sec)
3) Normality of Ooxalic Acid = 0.05N
4) Mean residense time in the reactor = t = V/ Fw (sec)

Observation Table:

Sr.No. Volume of Volume Outlet Time (t) E(t) t E(t) (t-tm)2

sample of Oxalic concentration seconds E(t)
V2 (ml) acid (ml) of NaOH C(t)
1
2
3
4
5

Calculations:
Plot concentration of NaOH (Ca) versus time and determine the area under the curve

Find E(t) = C(t) / C(t) dt
0

tm = Mean residense time = t. E(t) dt (min)
0

2 (Variance) = (t-tm)2 . t .dt (min)2
0

2 (skewness) = 2 / tm2 (dimensionless)

2 = 2/Pe 2/Pe2 (1-e-Pe)

By trial & error

Pe = ----------

Graphs : Plot the graph of C(t) v/s time

Plot the graph of E(t) v/s time
Plot the graph of t E(t) v/s time
Plot the graph of (t-tm)2 E(t) v/s time

Result:
Exercise No4: ( 2 Hours) 1 Practical
Dispersion Model (Packed Bed Reactor) - RTD
A] Aim: To determine RTD of a packed bed reactor and to find out peclet No.

Procedure:
1) Start the flow of water in the Packed bed reactor to build up the liquid level and to
achieve steady state
2) Measure the steady state flow rate
3) Take 10 ml of 1N NaOH in a syringe and inject it near the inlet of reactor and take
zero reading
4) Withdraw the sample at regular interval of time and titrate it against std. 0.05N oxalic
acid
5) Take 18 to 20 such readings
6) Plot graph of C(t) Vs time ,E(t) Vs time ,t.E(t) Vs time and (t-tm2).E(t) vs time using the
readings of observation table and calculate area under the curve of each graph.
Observations:
1) Normality of Oxalic acid = 0.05N
2) Flow rate = _________ml/sec
3) Normality of NaOH = 1N
Observation Table:

Sr.No. Time Vol of C(t) E(t) t.E(t) (t-tm)2.E(t)

(sec) t Oxalic gmole/lit
Acid (ml)
1
2
3
4
5

Calculations:
From graph calculate the values of

C(t) dt = _________
0

tm = Mean residense time = t. E(t) dt (min)
0

2 = (t-tm)2 .E(t) .dt (min)2
0
2 = 2 / tm2 (dimensionless)

2 = 2/Pe 2/Pe 2 (1 e-Pe)

Hence calculate peclet no (by trial and error ) from above equation.

Result:

Conclusion
Exercise No5: ( 2 Hours) 1 Practical
PFR -RTD
A] Aim: To study residence time distribution (RTD) in a plug flow reactor

Procedure:
1) Standardised solution of 0.05N oxalic acid is used for titration .
2) Fill one tank with water and & maitain steady state.
3) Take 10 ml of 1N NaOH in a syringe and inject all of it at one instant at inlet of the tank
and start the stopwatch simultaneously .
4) Take known volume of sample at the outlet of the reactor every ten seconds and
titrate this using 0.05N oxalic acid
5) Take at least 18 readings.

Observations:
1) Normality of NaOH = 1N
2) Flow rate of water = (ml/sec)
3) Normality of Ooxalic Acid = 0.05N
4) Mean residense time in the reactor = t = V/ Fw (sec)

Observation Table:

Sr.No. Volume of Volume Outlet Time (t) E(t) t E(t) (t-tm)2

sample of Oxalic concentration seconds E(t)
V2 (ml) acid (ml) of NaOH C(t)
1
2
3
4
5

Calculations:
Plot concentration of NaOH (Ca) versus time and determine the area under the curve

Find E(t) = C(t) / C(t) dt
0

tm = Mean residense time = t. E(t) dt (min)
0

2 (Variance) = (t-tm)2 . t .dt (min)2
0

2 (skewness) = 2 / tm2 (dimensionless)

2 = 2/Pe 2/Pe2 (1-e-Pe)

By trial & error

Pe = ----------

Graphs : Plot the graph of C(t) v/s time

Plot the graph of E(t) v/s time
Plot the graph of t E(t) v/s time
Plot the graph of (t-tm)2 E(t) v/s time

Result:
Exercise No6: ( 2 Hours) 1 Practical
Temperature Dependency
A] Aim: To estimate nature of temperature dependency of rate constant of ethyl acetate with NaOH in dilute
aqueous solution.

Chemicals required:
Ethyl acetate =0.1 N, Hcl, NaOH= 0.1 N, Std. Oxalic acid, phenolphthalein indicator, pipette,
burette etc.

Procedure:
1) Adjust the thermostat to obtain the constant temperature.
2) Take 25 ml of ethyl acetate solution in one standard flask of 100 ml and mount it in
the thermostat (flask 1)
3) Take 25 ml of 0.1 N NaOH solution in one standard flask of 100 ml and mount it in the
thermostat (flask 2)
4) Wait till thermal equilibrium is achieved.
5) Standardise NaOH solution using oxalic acid solution
6) Pour 25 ml of 0.1 N HCl into each of the flasks (1 & 2)
7) Carefully add contents of flask one to two and immediately transfer from two to one
.Place the conical flask in temperature bath and at the same time start the stop
watch
8) Pipette out 20 ml sample from the conical flask after 1.5 min and 2nd after 3 mints.
9) Back titrate against std 0.1 N HCl solution
10) Repeat the procedure for three different temperatures and intervals of at least 50 C

Observations:
Normality of Ethyl acetate solution =0.1N
Normality of Hcl solution = 0.1N
Normality of NaOH solution = 0.1N
Normality of Hcl for titration = N3= 0.1N
Volume of sample =V2= ______ml
Volume of Ethyl acetate =V1= ______ml

Observation Table:

Sr.No. Temperature Time Vol. Of CA 1/CA KC Ln KC 1/T K-1

(0K) Min HCl ml lit/gm.mole.min
1
2
3
4
5

Calculations:
CA = N1V1 N3V3 / V2

Slope = kc

1/CA

time (min)

KC = K0 C-E/RT
Slope = E/R

Ln KC

1/T

Result: The value of activation energy = _____ Kcal

Exercise No7: ( 2 Hours)
Two Continuous stirred tank reactor in series
A] Aim: To carry out saponification of ethyl acetate in given two CSTR in series and to determine the conversion and
to compare with single CSTR

Procedure:
1) Prepare 10 lit Standardized solution of 0.1 N ethyl acetate, 0.1 N NaOH
2) Prepare 1 lit Standardized solution of 0.1 N HCL
3) The observed tanks are filled with NaOH and ethyl acetate solution.
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) The mixture in the reactor is continuously stirred and the speed of the stirrer is
maintained at constant value.
7) Take 20 ml of 0.1 N HCL in a two flask and add 10 ml of reaction mixture from CSTR 1
to the flask 1 and 10 ml of reaction mixture from CSTR 2 to the flask 2.
8) Back titrate both mixture in the flask 1 & 2 with 0.1 N NaOH using phenolphthalein as
an indicator
9) Take five more samples from reacting streams (from CSTR 1 & CSTR 2)

Observations for CSTR 1:

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 =_________V21
8) Volume of HCL taken = _________V1
9) Volume of NaOH rundown in back titration = _________V3
10) Concentration of A1 (i.e. Ethyl Acetate) can be calculated as
CA1 = N1V1 N3V31 / V21
Observations for CSTR 2:
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 =_________V22
8) Volume of HCL taken = _________V1
9) Volume of NaOH rundown in back titration = _________V32
10) Concentration of A2 (i.e. Ethyl Acetate) can be calculated as
CA2 = N1V1 N3V31 / V21

Observation Table 1:
Sr.No. Flow Rate Flow Sample Sample NaOH NaOH Time
of ethyl Rate of Collected Collected V31 (ml) V32 (ml) (Sec.)
acetate NaOH From CSTR 1 from CSTR 2
(LPM) (LPM) V21 (ml) V22 (ml)

1
2
3
4
5
Prepare a observation Table 2 as follows:

Sr.No. CA0 CB0 CA1 CA2 CB1 CB2 XA1 XA1

1
2
3
4
5

Calculations for CSTR 1:

CA1 = N1V1 N3V31 / V21
F = FA+FB/2

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

N (EA) =Normality of ethyl acetate
CB1 = (CB0-CA0) +CA
Where CB0 = FB *N (NaOH) / FA+FB

And
Reaction rate rA =F (CA0-CA1)/V
XA1 = CA0-CA1/CA0
Prepare a Observation Table 2 as follows:

Calculations for CSTR 2:

CA2 = N1V1 N3V32 / V22
F = FA+FB/2

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

N (EA) =Normality of ethyl acetate
CB2 = (CB0-CA0) +CA
Where CB0 = FB *N (NaOH) / FA+FB

And
Reaction rate rA =F (CA0-CA2)/V
XA2 = CA0-CA2/CA0

Result:
1) Conversion in CSTR 1 is XA1 =
2) Conversion in CSTR 2 is XA2 =

Conclusion:
Exercise No8: ( 2 Hours) 1 Practical
Industrial Reactor
Aim: To study the different types of industrial reactors.

Theory: -

1) Packed Bed Reactor

2) Fluidized Bed Reactor

1) Packed Bed Reactor

A packed bed reactor is essentially a tubular reactor, which is packed with solid catalyst
particles. This type of reactor is constructed of either a single continuous tube or serial tubes in
parallel. The reactants enter at one end of reactor & the product leave from the other end
with a continuous variation in composition of reacting mixture in between. Heat transfer to or
from the reactor may be accomplished by means of a jacket or a shell & tube design. The
reactor tubes may be packs with catalyst pellet or inert solid. The tubular reactor finds
application in cases where back mixing of the reactor mixture in the flow direction is
undesirable. The large-scale gaseous reaction such as cracking of hydrocarbon, the
conversion of air to NO & the oxidation of No to NO2 are examples of the application of this
result.

Advantages & disadvantages of Packed Bed Reactor

Advantages-

1) Avoid degree of back mixing.

2) Avoid entrainment (i.e. carryover)
3) It usually produces highest conversion per reactor volume of any of the flow reactor.

Disadvantages

a. Ineffective heat transfer

b. Intra particle diffusion occurs.
c. It is difficult to control the temperature within the reactor & hot spots can color when
the reaction is exothermic.

3) Fluidized - Bed Reactor

This is a vertical cylindrical vessel containing fine solid particles that are either catalyst or
reactant. The fluid reactant stream is introduced at the bottom of the reactor at a rate such
that solids are floated in the fluid stream without being carried out of the system. Under this
condition the entire bed particles behave like a boiling liquid, which tends to equalize the
composition of reaction mixture & temperature throughout the bed. It is applied extensively to
solid-fluid reaction, such as the catalytic cracking of petroleum hydrocarbon, the conversion of
uranium oxide to uranium fluorides for reduction of some mineral ores and gasification of coal.

Advantages & Disadvantages of Fluidized Bed Reactor

Advantages

a. Effective heat transfer

b. The temperature is relatively uniform throughout thus avoiding heat effects.
c. Intra particle diffusion is avoided.
d. Can handle large amount of fuel & solid.
e. Ease of catalyst replacement or regeneration.

Disadvantages

a. Degree of back mixing is very large.

b. Attrition of catalyst with entrainment.
c. Less conversion.
d. High cost of reactor & catalyst regeneration equipment.
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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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.