Laboratory Manual for

3160506 –
Chemical Reaction Engineering I
 LUKHDHIRJI ENGINEERING COLLEGE,
MORBI

VISION

To provide quality engineering education and transforming students into professionally

competent and socially responsible human beings.

MISSION

1. To provide a platform for basic and advanced engineering knowledge to meet global
challenges.
2. To impart state-of-art know- how with managerial and technical skills.
3. To create a sustainable society through ethical and accountable engineering practices.
 LUKHDHIRJI ENGINEERING COLLEGE, MORBI
CHEMICAL ENGINEERING DEPARTMENT

VISION

To develop professionally competent & socially responsible chemical engineers by

providing quality education.
MISSION
1. To provide sound basic engineering knowledge to have a successful career in a
professional environment.
2. To develop skill sets among the students to make them professionally competent.
3. To cater ethically strong engineers who shall be able to improve the quality of life
and to work for sustainable development of society.
PEO’s
PEO-1 To impart knowledge and skills in students to make them professionally competent in chemical
process industries.
PEO-2 To motivate students for higher studies in technical and management fields.
PEO-3 To prepare students having soft skills along with leadership quality and management ability to
make them successful entrepreneurs.
PEO-4 To implant the ethical principle and norms of engineering practices in terms of health, safety, and
environmental context for the sustainable development of society.

PROGRAM OUTCOMES (POs)

Engineering Graduates will be able to:

1. Engineering knowledge: Apply the knowledge of mathematics, science, engineering fundamentals,

and an engineering specialization to the solution of complex engineering problems.
2. Problem analysis: Identify, formulate, review research literature, and analyze complex engineering
problems reaching substantiated conclusions using first principles of mathematics, natural sciences,
and engineering sciences.
3. Design/development of solutions: Design solutions for complex engineering problems and design
system components or processes that meet the specified needs with appropriate consideration for the
public health and safety, and the cultural, societal, and environmental considerations.
4. Conduct investigations of complex problems: Use research-based knowledge and research methods
including design of experiments, analysis and interpretation of data, and synthesis of the information
to provide valid conclusions.
5. Modern tool usage: Create, select, and apply appropriate techniques, resources, and modern
engineering and IT tools including prediction and modeling to complex engineering activities with an
understanding of the limitations.
6. The engineer and society: Apply reasoning informed by the contextual knowledge to assess societal,
health, safety, legal and cultural issues and the consequent responsibilities relevant to the professional
engineering practice.
7. Environment and sustainability: Understand the impact of the professional engineering solutions in
societal and environmental contexts, and demonstrate the knowledge of, and need for sustainable
development.
8. Ethics: Apply ethical principles and commit to professional ethics and responsibilities and norms of
the engineering practice.
9. Individual and team work: Function effectively as an individual, and as a member or leader in
diverse teams, and in multidisciplinary settings.
10. Communication: Communicate effectively on complex engineering activities with the engineering
community and with society at large, such as, being able to comprehend and write effective reports
and design documentation, make effective presentations, and give and receive clear instructions.
11. Project management and finance: Demonstrate knowledge and understanding of the engineering
and management principles and apply these to one’s own work, as a member and leader in a team, to
manage projects and in multidisciplinary environments.
12. Life-long learning: Recognize the need for, and have the preparation and ability to engage in
independent and life-long learning in the broadest context of technological change.

PSO
1) Apply the knowledge of chemical engineering to accomplish the contemporary need of chemical &
Allied Industries.
2) To execute the chemical engineering principle and modern engineering tools to design system by
considering safety, cost, health, legal, cultural and environmental aspects.
 Chemical Engineering Department
Laboratory Safety Rules
1 Behave in a responsible manner at all times in the laboratory.
2 Ask your teacher before preceding any activity.
3 Keep silence.
4 Do not touch any equipment, chemicals, or other materials in the
laboratory area until you are instructed to do so.
5 Perform only those experiments authorized by your teacher.
6 Do not eat food, drink beverages, or chew gum in the laboratory.
7 Always work in a well-ventilated area.
8 Work areas should be kept clean and tidy at all times.
9 Wash your hands after performing all experiments.
10 Dress properly during a laboratory activity. Long hair, dangling
jewellery, and loose or baggy clothing are a hazard in the laboratory.
11 Never look into a container that is being heated.
12 Obey safety rules.
13 After Completion of Experiments turn off equipment properly.
14 Drain Water After Compilation of Experiments.
15 Before Living the Laboratory turns Off Light/Fan.
 Undertaking of Ethics

1. I, hereby, promise to abide by the admissible rules and

regulations, concerning discipline, attendance, etc. of the
L.E.C.MORBI, and also to follow the Code of Conduct
prescribed for the Students of the Institute, as in force from
time to time and subsequent
changes/modifications/amendment made thereto. I
acknowledge that, the Institute has the authority for taking
punitive actions against me for violation and/or non-
compliance of the same.
2. I have performed all the experiments and their calculation
done myself.

Signature of Student

Enrolment of Student
 Index
Sr. Experiment Title of Experiment/Project Date of Teacher’s Remarks/
No. No./Assignment Submission sign Marks
No./Project work Obtained

Must complete and submit on or before given date

1 Experiment 1 To prepare calibration chart for

Concentration Vs. Conductivity or
TDS.

2 Experiment 2 To measure the kinetics of a

reaction between ethyl acetate
and sodium hydroxide under
condition of equimolal
concentration at room
temperature using integral
method of analysis.

3 Experiment 3 To determine the kinetics of the

reaction between excess ethyl
acetate and sodium hydroxide at
room temperature by the
differential method of analysis.

4 Experiment 4 To determine the activation

energy of the reaction between
ethyl acetate and sodium
hydroxide using Arrhenius
Equation.

5 Experiment 5 Verify performance equation of

PFR and predict conversion using
known rate expression.

6 Experiment 6 Study characteristics of CSTR and

predict conversion using known
rate expression.

7 Experiment 7 Compare performance of reactor

in series. For example, PFR + CSTR

8 Experiment 8 Compare performance of single

CSTR and multiple CSTR in series

9 Experiment 9 Compare performance of PFR and

PFR with recycle.

10 Experiment 10 Residence Time Distribution (RTD)

studies using pulse input in PFR.
 11 Experiment 11 Residence Time Distribution (RTD)
studies using pulse input in CSTR.

Open Ended Project: Fabrication and Poster Preparation (A1 size) for following topics

1 A1 batch Fabrication CSTR reactor setup

and its performance (one tank 400
ml reaction volume)

2 A2 batch Fabrication PFR reactor setup and

its performance (one pipe of 400
ml reaction volume)

3 A3 batch Fabrication Tank in Series setup

and its performance (1 tank of 600
ml reaction volume, 2 tanks of 300
ml each of reaction volume and 3
tanks of 200 ml each of reaction
volume)

4 A4 batch Fabrication and Performance of

CSTR followed by PFR in Series
setup

5 A5 batch Fabrication of setup and

Performance of PFR without and
with Recycle (R)
List of Equipments and Aim of experiments for
3160506 Chemical Reaction Engineering-I Laboratory
Time: Dec 2020 - April 2021
SR. NAME OF AIM OF EXPIREMENT PO PSO
CO
NO. INSTRUMENT
To prepare calibration chart for
1 Batch Reactor Concentration Vs. Conductivity or TDS. PO1,2,8,9,12 PSO1

To measure the kinetics of a reaction

between ethyl acetate and sodium
2 Batch Reactor hydroxide under condition of equimolal 31605 PO1,2,8,9,12 PSO1
ethyl acetate at room temperature using 06.1
integral method of analysis.

To determine the kinetics of the reaction

between excess ethyl acetate and sodium 31605
3 Batch Reactor hydroxide at room temperature by the 06.1 PO1,2,8,9,12 PSO1
differential method of analysis.

4 Batch Reactor To determine the activation energy of the 31605 PO1,2,8,9,12 PSO1
reaction between ethyl acetate and 06.1
 sodium hydroxide using Arrhenius
Equation.

Verify performance equation of PFR and

5 PFR predict conversion using known rate 31605 PO1,2,8,9,12 PSO1
expression. 06.2

Study characteristics of CSTR and predict 31605

6 CSTR conversion using known rate expression. 06.2 PO1,2,8,9,12 PSO1

Compare performance of reactor in series. 31605

7 PFR + CSTR For example, PFR + CSTR PO1,2,8,9,12 PSO1
06.2
Compare performance of single CSTR 31605
8 CSTR and multiple CSTR in series PSO1,
06.2 PO1,2,8,9,12 2
9 Compare performance of PFR and PFR 31605
PFR with recycle. PSO1,
06.3 PO1,2,8,9,12 2
Residence Time Distribution (RTD) 31605
10 PFR studies using pulse input in PFR. PSO1,
06.4 PO1,2,8,9,12 2
CSTR Residence Time Distribution (RTD) 31605
11 studies using pulse input in CSTR. PO1,2,8,9,12 PSO1
06.4

Open Ended Project: Fabrication and Poster Preparation (A1 size) for following topics
Design and Fabrication CSTR reactor 31605
setup and study its performance (one tank 06.2
1 CSTR 500 ml reaction volume) by changing and31 PO1,2,8,9,12 PSO1
various reaction parameters. 60506
.3
Design and Fabrication PFR reactor setup 31605
(one pipe of 500 ml reaction volume) and 06.2
2 PFR study its performance by changing and31 PO1,2,8,9,12 PSO1
various reaction parameters. 60506
.3
Design and Fabrication Tank in Series
setup and its performance (1 tank of 1500
31605
ml reaction volume, 2 tanks of 750 ml 06.2
3 CSTR in series each of reaction volume and 3 tanks of and31 PO1,2,8,9,12 PSO1
500 ml each of reaction volume) and 60506
study its performance by changing .3
various reaction parameters.

Design and Fabrication of setup of CSTR 31605

followed by PFR (and vice versa) in 06.2
4 CSTR and PFR Series and study its performance by and31 PO1,2,8,9,12 PSO1
changing various reaction parameters. 60506
.3
5
Experiment No. Date:
OBJECTIVE: To prepare calibration chart for NaOH solution.
APPARTUS: Beaker, conical flask, measuring cylinder, weighing balance, conductometer.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 50 ml NaOH solution (with regular tap water) having concentration 0.05 N.

● Measure its conductivity/TDS.

● Add sufficient water in above solution. Calculate new concentration and measure its
conductivity/TDS.
● Repeat this procedure till 0.005 N for NaOH solution.

OBSERVATION TABLE:
Sr. No. Concentration of NAOH (CA) Conductivity/TDS meter
reading (ms/cm or ppm)
(mol L-1 )
Chart: Prepare chart of Concentration Vs. Conductivity or TDS for above values.
Experiment No. Date:
OBJECTIVE: To measure kinetics of reaction between equimolal ethyl acetate and sodium
hydroxide at room temperature by integral method of analysis (CO-1).
APPARTUS: Beaker, conical flask, measuring cylinder, weighing balance, conductivity
meter/TDS meter.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 50ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 50ml of 0.05 N ethyl acetate solution using RO water.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Take 50ml 0.05 N sodium hydroxide solutions into 250ml beaker and start stirring.

● Add 50ml 0.05N ethyl acetate solution in sodium hydroxide solution and measure
conductivity at t=0 of mixture.
● Note down reading of conductivity/TDS meter on regular internal of 20 sec till conductivity
meter reach steady state.
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

Sr. No Time, sec Conductivity/TDS reading Concentration (mol L-1 s-1)

(Take only 10 representative (From Calibration Chart)
values from record book)
CALCULATIONS:

Sr. No Time, sec CA , -ln (1-XA) 1/CA

Concentration (mol
L-1 s-1)

RESULTS:
 ● The order of the reaction is is_______________ and

● rate expression is…..

-rA =
CONCLUSION:
Experiment No. Date:
OBJECTIVE: To measure kinetics of reaction between access ethyl acetate and sodium hydroxide
at room temperature by differential method of analysis (CO-1).
APPARTUS: Beaker, conical flask, measuring cylinder, weighing balance, conductivity
meter/TDS meter
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 50ml of 0.02 N sodium hydroxide solution using RO water.

● Prepare 50ml of 0.08 N ethyl acetate solution using RO water.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Take 50ml 0.02 N sodium hydroxide solutions into 250ml beaker and start stirring.

● Add 50ml 0.08N ethyl acetate solution in sodium hydroxide solution and measure
conductivity at t=0 of mixture.
● Note down reading of conductivity/TDS meter on regular internal of 20 sec till conductivity
meter reach steady state.
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

Sr. No Time, sec Conductivity/TDS reading Concentration (mol L-1 s-1)

(Take only 10 representative (From Calibration Chart)
values from record book)
CALCULATIONS:

Sr. No Time, sec CA , -rA = -dCA/dt

Concentration (mol
L-1 s-1)

RESULTS:
 ● The order of the reaction is is_______________ and

● rate expression is…..

-rA =
CONCLUSION:
Experiment No. Date:
OBJECTIVE: To find activation energy of reaction between equimolal ethyl acetate and sodium
hydroxide (CO-1).
APPARTUS: Beaker, conical flask, measuring cylinder, weighing balance, conductivity
meter/TDS meter
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 50ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 50ml of 0.05 N ethyl acetate solution using RO water.

● Prepare constant temperature water bath.

● Increase and maintain temperature T1 (30 oC) of water bath.

● Increase and maintain temperature of both solutions separately to T1 (30 oC) by keeping
both solutions in constant water bath.
● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Take 50ml 0.05 N sodium hydroxide solutions into 250ml beaker and start stirring.

● Add 50ml 0.05 N ethyl acetate solution in sodium hydroxide solution and measure
conductivity at t=0 of mixture.
● Make sure temperature of reaction mixture must remain constant at T1 (30 oC).

● Note down reading of conductivity/TDS meter on regular internal of 20 sec till conductivity
meter reach steady state.
● After completion of 1st set of experiment, clean all beakers and other glasswares.

● Repeat the same experiment at other two temperatures, T2 (40 oC) and T3 (50 oC).

● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

 ● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

Sr. Temperature T1 ______, oC Temperature T2 ______, oC Temperature T3 ______, oC

No
Time, s Conducti Concentr Time, s Conducti Concentr Time, s Conducti Concentr
vity/TDS ation vity/TDS ation vity/TDS ation
(mol L-1 (mol L-1 (mol L-1
s-1) s-1) s-1)

10

CALCULATIONS:

Sr. Temperature T1 ______, oC Temperature T2 ______, oC Temperature T3 ______, oC

No
Time, s Concentr 1/CA Time, s Concentr 1/CA Time, s Concentr 1/CA
ation ation ation
(mol L-1 (mol L-1 (mol L-1
s-1) s-1) s-1)

9
 10

Plot graph of 1/CA Vs t and find value of k

Sr. No Temperature, 0C k (mol-1 L1 s-1)

RESULTS:

● Activation Energy of reaction _______________ and

● Frequency factor _________________

CONCLUSION:
Experiment No. Date:
OBJECTIVE: To verify performance equation of PFR and predict conversion using known rate
expression (CO-2).
APPARTUS: Beaker, PFR setup, measuring cylinder, weighing balance, conductivity meter/TDS
meter.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 500 ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 500 ml of 0.05 N ethyl acetate solution using RO water.

● Prepare PFR reactor setup and make sure all piping connections are done properly.

● Measure total volume of PFR reactor.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Set flow of both solution 4 ml per sec (individual flow 4 ml/sec, total flow of both solution
8 ml/sec).
● Start flow of both solutions in reactor together. Make sure both solutions must have same
flow rate while entering in the PFR.
● Allow some time to reach steady state in reactor.

● Once flow reaches at steady state condition, note down reading of conductivity/TDS meter
of exit fluid on regular internal of 20 sec. Meter reading must be almost constant.
● Repeat the experiment by changing flow of both solution (as given in cal part of excel
sheet).
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

● Total volume of PFR reactor = _______ N

 Sr. No Volume metric Space time, τ Conductivity/TDS Concentration (mol L-1 s-
1
flow, ml/sec sec reading (Take only 10 ) (From Calibration
representative values Chart)
from record book)

CALCULATIONS:

V/FA0 = τ/CA0 = Integration(dCA/-rA)

CA0 = __________

V = _________

Rate constant of reaction, k = ___________

Sr. No Space time, τ sec CA , Concentration (mol L-1 s-1)

Experimental Value Calculated Value based on performance

equation

Volume of reactor required to achieve 90% conversion = ________

RESULTS:

● For 400 ml volume PFR and ____ ml per sec total feed flow rate, 90% conversion can be
achieved with ______ sec space time .

CONCLUSION:
Experiment No. Date:
OBJECTIVE: Study characteristics of CSTR and predict conversion using known rate expression.
(CO-2).

APPARTUS: Beaker, CSTR setup, measuring cylinder, weighing balance, conductivity meter/TDS
meter.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 500 ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 500 ml of 0.05 N ethyl acetate solution using RO water.

● Prepare CSTR reactor setup and make sure all piping connections are done properly.

● Measure total volume of CSTR reactor.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Set flow of both solution 20 ml per min (individual flow 20 ml/min, total flow of both
solution 40 ml/min).
● Start flow of both solutions in reactor together. Make sure both solutions must have same
flow rate while entering in the reactor.
● Allow some time to reach steady state in reactor.

● Once flow reaches at steady state condition, note down reading of conductivity/TDS meter
of exit fluid on regular internal of 10 sec. Meter reading must be almost constant.
● Repeat the experiment by changing flow of both solution 20 ml/s, 13.5 ml/s, 10 ml/s and 8
ml/s and measure concentration.
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

 ● Total volume of PFR reactor = _______ N

Sr. No Volume metric Space time, τ Conductivity/TDS Concentration (mol L-1 s-

1
flow, ml/sec sec reading (Take only 10 ) (From Calibration
representative values Chart)
from record book)

CALCULATIONS:

V/FA0 = τ/CA0 = (ΔCA/-rA)

CA0 = __________

V = _________

Rate constant of reaction, k = ___________

Sr. No Space time, τ sec CA , Concentration (mol L-1 s-1)

Experimental Value Calculated Value based on performance equation

Volume of reactor required to achieve 90% conversion = ________

RESULTS:

● For 400 ml volume CSTR and ____ ml per sec total feed flow rate, 90% conversion can be
achieved with ______ sec space time.
CONCLUSION:
Experiment No. Date:
OBJECTIVE: Compare performance of reactor in series for example, PFR + CSTR and CSTR
+PFR (CO-2)
APPARTUS: Beaker, CSTR setup, PFR setup, measuring cylinder, weighing balance, conductivity
meter/TDS meter.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 1000 ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 1000 ml of 0.05 N ethyl acetate solution using RO water.

● Prepare PFR + CSTR reactor setup and make sure all piping connections are done properly.

● Measure total volume of PFR and CSTR reactor.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Set flow of both solution 20 ml per min (individual flow 20 ml/min, total flow of both
solution 40 ml/min).
● Start flow of both solutions in PFR together. Make sure both solutions must have same flow
rate while entering in the reactor. Outlet of PFR must enter in CSTR. Keep minimum
possible piping to reduce conversion in piping.
● Allow some time to reach steady state in both reactors.

● Once flow reaches at steady state condition, note down reading of conductivity/TDS meter
of exit fluid from PFR and CSTR on regular internal of 10 sec. Meter reading must be
almost constant.
● Repeat the experiment by changing sequence of reactors, for example now sequence must
be CSTR + PFR. Keep all other parameters constant like flow of both solution at same flow
rate as in previous case, 20 ml/s indvidually and measure concentration.
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

 ● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

● Total volume of PFR reactor = _______ N

First Experiment (PFR + CSTR):

Sr. Volume Space PFR exit PFR exit CSTR exit CSTR exit
No metric time, τ sec Conductivity/TDS Concentration Conductivity/T Concentrati
flow, reading (only one (mol L-1 s-1) DS reading on (mol L-1
ml/sec final Steady State (only one final s-1)
reading) Steady State
reading)

Second Experiment (CSTR+PFR):

Sr. Volume Space CSTR exit CSTR exit PFR exit PFR exit
No metric time, τ sec Conductivity/TD Concentration Conductivity/TD Concentrati
flow, S reading (only (mol L-1 s-1) S reading (only on (mol L-1
ml/sec one final Steady one final Steady s-1)
State reading) State reading)

CALCULATIONS:

Calculate theoretically concentration using performance equation in both cases for both reactors.

V/FA0 = τ/CA0 = (ΔCA/-rA)

CA0 = __________

V = _________

Rate constant of reaction, k = ___________

Sr. Space Case 1Exit CA, Concentration (mol L-1 s-1) Case 2Concentration Values, CA,
No time, τ Concentration (mol L-1 s-1)
sec
PFR, CA CSTR, CA CSTR, CA PFR, CA

Experime Theoreti Experi Theoreti Experi Theoreti Experi Theor

ntal Value cal mental cal mental cal mental etical
Value Value Value Value Value Value Value
RESULTS:
Final conversion achieved in PFR + CSTR = ______
Final conversion achieved in CSTR + PFR = ______

CONCLUSION:
Experiment No. Date:
OBJECTIVE: Compare performance of single CSTR and multiple CSTR in series (CO-2).
APPARTUS: Beaker, CSTR setup, CSTR in Series setup, measuring cylinder, weighing balance,
conductivity meter/TDS meter.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 1000 ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 1000 ml of 0.05 N ethyl acetate solution using RO water.

● Prepare CSTR reactor setup and make sure all piping connections are done properly.

● Measure total volume of CSTR reactor.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Set flow of both solution 20 ml per min (individual flow 20 ml/min, total flow of both
solution 40 ml/min).
● Start flow of both solutions in reactor together. Make sure both solutions must have same
flow rate while entering in the reactor.
● Allow some time to reach steady state in reactor.

● Once flow reaches at steady state condition, note down reading of conductivity/TDS meter
of exit fluid on regular internal of 10 sec. Meter reading must be almost constant.
● Repeat the experiment with three equal volume CSTR in series. Make sure that volume of
single CSTR and total volume of three CSTR must be equal (For example single CSTR
having volume of 600 ml, three CSTR in series must have 200 ml for each and total volume
600 ml).
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml..

● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

 ● Total volume of PFR reactor = _______ N

Single CSTR:

Sr. No Volume metric Space time, τ Conductivity/TDS Concentration (mol L-1 s-

1
flow, ml/sec sec reading )

Three CSTR in series:

Sr. No Volume Space CSTR 1 CSTR 2 CSTR 3

metric time, τ sec
flow,
ml/sec

Cond./ Conce Cond./ Conce Cond./ Conce

TDS ntratio TDS ntratio TDS ntratio
reading n (mol readin n (mol readin n (mol
L-1 s-1) g L-1 s-1) g L-1 s-1)

CALCULATIONS:

CA0 = __________

V = _________

Rate constant of reaction, k = ___________

For single CSTR, V/FA0 = τ/CA0 = (ΔCA/-rA)

For CSTR in series,

Sr. No Space Single CSTR CSTR in Series

time, τ sec
CSTR 1 CSTR 2 CSTR 3

Experi Theor Experi Theor Experi Theor Experi Theor

menta etical mental etical menta etical menta etical
l CA Value, CA l CA l CA
Value, Value, Value,
 CA CA CA CA

RESULTS:

● Single CSTR concentration ______ mol/l

● Final exit concentration of three CSTR in series ____ mol/l

CONCLUSION:
Experiment No. Date:
OBJECTIVE: Compare performance of PFR and PFR with recycle (CO-3)
APPARTUS: Beaker, PFR setup, PFR with recycle setup, measuring cylinder, weighing balance,
conductivity meter/TDS meter.
CHEMICALS: Water, ethyl acetate, NaOH.

PROCEDURE:

● Prepare 1000 ml of 0.05 N sodium hydroxide solution using RO water.

● Prepare 1000 ml of 0.05 N ethyl acetate solution using RO water.

● Prepare PFR reactor setup and make sure all piping connections are done properly.

● Measure total volume of PFR reactor.

● Before starting reaction, measure conductivity/TDS of sodium hydroxide solution.

● Set flow of both solution 4 ml per sec (individual flow 4 ml/sec, total flow of both solution
8 ml/sec).
● Start flow of both solutions in reactor together. Make sure both solutions must have same
flow rate while entering in the PFR.
● Allow some time to reach steady state in reactor.

● Once flow reaches at steady state condition, note down reading of conductivity/TDS meter
of exit fluid on regular internal of 20 sec. Meter reading must be almost constant.
● Repeat the experiment with PFR with recycle reactor setup and make sure all piping
connections are done properly. Keep the concentration and other parameters same as
previous experiment. Measure final concentration after reaching steady state.
● After completion of experiment wash all glassware properly and keep all glassware,
chemicals and instrument in proper place.

OBSERVATION:

● Concentration of NaOH solution prepared = _____N

● Volume of NaOH solution taken = _____ ml

● Volume of Ethyl Acetate solution taken = _____ ml

● Initial concentration of NaOH in reaction mixture (at t=0 sec) = ______ N

● Total volume of PFR reactor = _______ N

 ● Volume metric flow= _________ ml/sec

● Space time, τ = _________ sec

Sr. Recycle PFR Without recycle PFR with recycle

No Ratio, R

Conductivity/ Concentration Conductivity Concentration

TDS reading (mol L-1 s-1) /TDS reading (mol L-1 s-1)

1 0

2 0.5

3 1

4 2

5 3
CALCULATIONS:

CA0 = __________

Volume metric flow= _________ ml/sec

Space time, τ = _________ sec

V = _________

Rate constant of reaction, k = ___________

For PFR without any recycle,

V/FA0 = τ/CA0 = Integration(dCA/-rA)

For PFR with recycle R,

Sr. Recycle PFR Without recycle PFR with recycle

No Ratio, R

Experimental Theoretical CA Experimental Theoretical CA

Value, CA Value, CA

1 0

2 0.5
3 1

4 2

5 3

RESULTS:

● Conversion in PFR without recycle is ________

● Conversion in PFR with R=3 is ________

● As R increases, conversion _________

CONCLUSION:
Experiment No:
RTD STUDIES IN PLUG FLOW REACTOR (CO-4)
OBJECTIVE: Residence Time Distribution (RTD) studies using pulse input in PFR.
CHEMICALS: NaCl salt, KMNO4, water.
APPARATUS: Plug flow reactor, TDS/conductivity meter.
PROCEDURE:
Adjust flow meter and conductivity meter. Check accuracy and calibration using standard samples.
Prepare setup for straight pipe reactor. Start water flow through straight pipe reactor and allow to
reach steady state. Measure the time taken by using dummy tracer 1N KMNO 4. A solution of
around 50 ml of the tracer (x N NaCl/NaOH) is injected through a syringe of the inlet of reactor as
quickly as possible & simultaneously a stopwatch is started. At regular intervals of time measure
conductivity of exit stream using calibrated conductivity meter. Measure the steady state flow rate
of water.
Change flow rate (increase or decrease compared to earlier flow) and repeat the complete
experiment for four different water flow rates.
Volume of reactor ___________
Volumetric flow rate of water ____________
Tracer concentration ______ and volume injected ________

Observation Table:
Time, TDS/
Sr.
t, Conduc
No mol/
Sec tivity
.
reading L
1
2
3
4
5
6
7
8
9
10

Calculations:
(i) = _________
Q (graphical) = Area under the curve of C vs t graph =

(ii) E=C /Q
E graphical: C(t)/ Q(graphical)

Calculations (Cont.:

(iii) = ____________
∞
− ∫ t .E(t ).dt
t graphical from 0 =___________.

(iv)

F= ∑ Ei Δti
t
Fgraphical=∫ E(t )dt
0

Graphs:
C v/s t
E v/s t
F v/s t

Result:

Conclusion:
QUIZ:
1. Discuss factors which are responsible for deviation from ideal plug flow contacting
pattern in real scenario.
2. Qualitatively draw exit age distribution curve for ideal plug flow reactor. Comment on
nature of this curve.
3. Discuss importance of RTD studies in chemical reaction engineering.
Experiment No: Date:
RTD STUDIES IN CSTR (CO-4)
OBJECTIVE: Residence Time Distribution (RTD) studies using pulse input in CSTR
CHEMICALS: NaOH, KMNO4, water.
APPARATUS: CSTR, TDS/conductivity meter.
PROCEDURE:
Adjust flow meter and TDS/conductivity meter. Check accuracy and calibration using standard
samples. Prepare setup for continuous stirred tank reactor (CSTR). Start water flow through CSTR
and allow to reach steady state. Measure the time taken by using dummy tracer 1N KMNO 4. A
solution of around x ml of the tracer (x N NaOH or x N NaCl) is injected through a syringe of the
inlet of reactor as quickly as possible & simultaneously a stopwatch is started. At regular intervals
of time measure conductivity of exit stream using calibrated conductivity/TDS meter. Measure the
steady state flow rate of water.
Change flow rate (increase or decrease compared to earlier flow) and repeat the complete
experiment for four different water flow rates.
Volume of reactor ___________.
Volumetric flow rate of water ____________
Tracer concentration ______ and volume injected ________

Observation Table:
Time, Conduc
Sr. t,
tivity mol/
No. Sec
reading L
1
2
3
4
5
6
7
8
9
10

Calculations:
(i) = _________
Q (graphical) = Area under the curve of C vs t graph =

(ii) E=C /Q
E graphical: C(t)/ Q(graphical)

Calculations (Cont.:

(iii) = ____________
∞
− ∫ t .E(t ).dt
t graphical from 0 =___________.

(iv)

F= ∑ Ei Δti
t
Fgraphical=∫ E(t )dt
0

Graphs:
C v/s t
E v/s t
F v/s t
Eθ v/s θ
Fθ v/s θ
Result:

Conclusion:

QUIZ:
1. Discuss factors which are responsible for deviation from ideal mixed flow contacting
pattern in real scenario.
2. Qualitatively draw exit age distribution curve for ideal CSTR. Comment on nature of
this curve.
3. Suggest some non-ideal flow pattern present in CSTR and also suggest remedies to
remove the same.
Date:
Experiment No:
RTD STUDIES IN PLUG FLOW REACTOR WITH STEP INPUT SIGNAL (CO-1)
OBJECTIVE: Residence Time Distribution (RTD) studies using STEP input in PFR.
CHEMICALS: NaCl salt/NaOH, KMNO4, water.
APPARATUS: Plug flow reactor, TDS/conductivity meter.
PROCEDURE:
Adjust flow meter and conductivity meter. Check accuracy and calibration using standard samples.
Prepare setup for straight pipe reactor. Start water flow through straight pipe reactor and allow to
reach steady state. Prepare y ml x n NaCl salt/KMnO4 solution and adjust its flow and measure its
flow. Start adding tracer flow inside the PFR. Measure the time taken by tracer. At regular
intervals of time measure TDS/conductivity of exit stream using calibrated TDS/conductivity
meter. Measure the steady state flow rate of water and tracer flow.
Change flow rate (increase or decrease compared to earlier flow) and repeat the complete
experiment for four different water flow rates.
Volume of reactor ___________
Volumetric flow rate of water ____________
Tracer concentration ______ and volumetric flow of tracer ________

Observation Table:
Time, TDS/ E
Sr.
Conduc
No t, mol/ F
tivity
.
Sec reading L
1
2
3
4
5
6
7
8
9
10
Calculations:

(i) = _________
Q (graphical) = Area under the curve of C vs t graph =

Graphs:
C v/s t
E v/s t
F v/s t

Result:

Conclusion:

QUIZ:
1. Discuss advantage and disadvantages of STEP input over PULSE input signal.
Experiment No: Date:

RTD STUDIES IN PACKED BED REACTOR (CO-1)

Objective: Residence Time Distribution (RTD) studies using pulse input in packed bed reactor.

Apparatus: Packed bed reactor setup, Tracer Injection device, Measuring Cylinder (250 ml),
Conductivity meter, Stop watch.

Chemicals: Water, NaOH, HCl, KMNO4

Theory: Residence Time Distribution (RTD) is very important for parameter to study non-ideality
of the any system. Having non-ideal flow behavior, performance of any system can be improved by
removing such non-ideality.
Write various types of non-idealities present in packed bed reactor. Also write to measure such non-
ideality and parameter to be measured and give suggestions to rectify such non-idealities.

Procedure:

● Adjust flow meter and conductivity meter.

● Check accuracy and calibrate using standard samples.

● Prepare setup for packed bed reactor with all necessary accessories.

● Start minimum water and gas flow through packed bed reactor and allow to reach steady
state.
● Measure the time taken by using dummy tracer 1N KMNO4.

● A solution of around 50 ml of the tracer (x N NaOH) is injected through a syringe of the

inlet of reactor as quickly as possible & simultaneously a stopwatch is started.
● At regular intervals of time measure conductivity of reaction mixture using calibrated
conductivity meter. Measure the steady state flow rate of H2O.
Change flow rate (increase or decrease compared to earlier flow) and repeat the complete
experiment for four different water flow rates.

Volume of reactor ___________

Volumetric flow rate of reactor ___________

Observation Table:
 Time,
Sr. Conduc
No t, tivity mol/
. reading L
Sec
1
2
3
4
5
6
7
8

Calculations:

(i) = _________
Q (graphical) = Area under the curve of C vs t graph =

(ii) E=C /Q
E graphical: C(t)/ Q(graphical)

Calculations (Cont.:

(iii) = ____________
∞
− ∫ t .E(t ).dt
t graphical from 0 =___________.
(iv)
F= ∑ Ei Δti
t
Fgraphical=∫ E(t )dt
0

Graphs:
C v/s t
E v/s t (both practical and graphical values)
F v/s t (both practical and graphical values)
Result:

Conclusion:

Quiz:
1. How can you prove that flow inside packed column is ideal plug flow behavior?
2. Draw inlet and outlet tracer concentration profile (hypothetical) for ideal plug flow
behavior? You can use different flow pattern of tracer like impulse input or step input or any
type of input.
3. Which type of non-idealities present in packed tower you have used? Just list out the
parameters.