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Cre Lab

This document provides information about a chemical reaction engineering lab at Hindusthan College of Engineering and Technology. It outlines the course outcomes, program outcomes, and experiment procedures for determining the rate constant and kinetics for the saponification reaction of ethyl acetate and sodium hydroxide in a continuous stirred tank reactor.
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0% found this document useful (0 votes)
26 views42 pages

Cre Lab

This document provides information about a chemical reaction engineering lab at Hindusthan College of Engineering and Technology. It outlines the course outcomes, program outcomes, and experiment procedures for determining the rate constant and kinetics for the saponification reaction of ethyl acetate and sodium hydroxide in a continuous stirred tank reactor.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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HINDUSTHAN COLLEGE OF ENGINEERING AND

TECHNOLOGY
(An Autonomous Institution, Approved by AICTE, New Delhi, Affiliated to Anna University, Chennai,)

DEPARTMENT OF CHEMICAL ENGINEERING

CHEMICAL REACTION ENGINEERING LAB

LABORATORY MANUAL

NAME OF THE FACULTY SIGNATURE

PREPARED BY Ms. KALPANA V P

APPROVED BY Dr. SEENUVASAN

NAME OF THE STUDENT :

REGISTER NO :
Course Outcomes (COs):
Upon successful completion of this course, the student will be able to:

CO1- Understanding the concepts of different types of reactors.


CO2- Ability to apply the reaction order to determine the kinetics and residence time.
CO3- Ability to analyze the use of reactors for particular industry by using the reaction rate. CO4-
Ability to select the appropriate CSTR and PFR.
CO5- Ability to design the reactors.

Programme Outcomes and Programme Specific Outcomes

Program Outcomes Descriptions


PO1 Engineering Apply the knowledge of mathematics, science, engineering
knowledge fundamentals, and an engineering specialization to thesolution of
complex engineering problems.
PO2 Problem analysis Identify, formulate, research literature, and analyze complex
engineering problems reaching substantiated conclusions using
first principles of mathematics, natural sciences, and engineering
sciences.
PO3 Design/developmentof Design solutions for complex engineering problems and design
solutions system components or processes that meet the specified needs with
appropriate consideration for the publichealth and safety, and the
cultural, societal, and environmental considerations.
Use research-based knowledge and research methods including
PO4 Conduct investigations design of experiments, analysis and interpretation of data, and
of complex problems synthesis of the information to provide valid conclusions.

PO5 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.
PO6 The engineer and Apply reasoning informed by the contextual knowledge to assess
society societal, health, safety, legal and cultural issues and the consequent
responsibilities relevant to the professional engineering practice
Understand the impact of the professional engineering solutions in
PO7 Environment and societal and environmental contexts, and demonstrate the
sustainability knowledge of, and need for sustainable development.

PO8 Ethics Apply ethical principles and commit to professional ethics


and responsibilities and norms of the engineering practice.
PO9 Individual and team Function effectively as an individual, and as a member orleader
work in diverse teams, and in multidisciplinary settings.
PO10 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 effectivepresentations, and give and
receive clear instructions.
PO11 Project management and Demonstrate knowledge and understanding of theengineering and
finance 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
PO12 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.

Programme Educational Objectives:

PEO 1: Participate as leaders in their fields of expertise and in activities that support service
and economic development nationally and throughout the world.
PEO 2: Pursue continued life-long learning through professional practice, research and training
programs in the field of chemical engineering and science.
PEO 3: Solve real-life problems in a broad perspective to fulfill ethical, economic,
environmental and social responsibilities.
CHEMICAL REACTION ENGINEERING LABORATORY

Name: I.D. No:

CONTENTS

Sl. Date of
Date Particulars Signature
No. submission

5
EXP NO.

DATE:

Kinetic studies in CSTR (Equimolar)

Aim
To determine the rate constant and the kinetics for saponification of equimolar quantity of ethyl acetate and
sodium hydroxide in a continuous stirred tank reactor.

Apparatus required

Pipette
Burette
Standard measuring jar-250ml beaker
Conical flask
Stop watch
MFR setup.
Chemicals required
Sodium hydroxide (NaOH) Ethyl acetate
(CH3COOC2H5)Acetic acid (CH3COOH)
Water (H2O)
Hydrochloric acid (Hcl) Phenolphthalein
indicator
Theory
A mixed flow reactor or a CSTR is operated at steady state. There is no accumulation. The total mass
flow rate at which the reactants are fed to the reactor is equal to the mass flow rate at which the products
are withdrawn from the reactor. Therefore, the properties in the CSTR do not change with time. The
concentration of reactants drops to the outlet concentration immediately on entering the CSTR. The
concentration of the material does not vary with time. Since the reactor is well mixed, the concentration
throughout the reactors is uniform i.e. there is no spacial variation in concentration in the reactors at any
time. Thus the rate of reaction in a CSTR is constant throughout the reactor at fixed temperature. Since
there is a concentration gradient along the reactor. In flow reactor, space time and residence time
are important parameter. The residence time can be varied either by varying the flow rate and keeping
the volume of reactor constant (or) vice-versa.

As the residence time decreases, the conversion decreases for liquid phase reaction i.e. for reaction
with constant density. The space time which is the time required to process one reactor volume of fluid
is equal to the mean residence time.
The reaction between sodium hydroxide and ethyl acetate can be represented as,
NaOH + CH3COOC2H5  CH3COONa + C2H5OH

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑟𝑒𝑎𝑐𝑡𝑜𝑟


Space time, =
𝑇𝑜𝑡𝑎𝑙 𝑉𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜w 𝑟𝑎𝑡𝑒

−𝑟𝐴 = 𝑘𝐶𝐴𝐶𝐵 = 𝑘𝐶𝐴0(1 − 𝑋𝐴) 𝐶𝐵0(𝑀 − 𝑋𝐴)

𝐶𝐴0
𝑀= = 1 (𝑓𝑜𝑟 𝐸𝑞𝑢𝑖𝑚𝑜𝑙𝑎𝑟)
𝐶𝐵0

−𝑟𝐴 = 𝑘CA2 = 𝑘𝐶2𝐴0 ( 1 − 𝑋𝐴)2

The design equation for MFR is,


𝑉
𝑉 𝑋𝐴 𝜏
= =
𝐹𝐴𝑂 −𝑟𝐴 𝐶𝐴𝑂
Procedure
1. The solution of sodium hydroxide, hydrochloric acid, acetic acid and ethylacetate of
required strength are prepared.
2. Sodium hydroxide and hydrochloric acid solutions are standardized.
3. The storage reservoirs were filled with -------------- lit of sodium hydroxide and lit of ethyl
acetate solution.
4. The required flow rates of sodium hydroxide and ethyl acetate were adjusted using rotameter
such that the flow rate of both sodium hydroxide and ethyl acetate were same (for feeding
on equimolar quantity of sodium hydroxide and ethyl acetate).
5. Steady state conditions were allowed to be obtained. i.e. outlet flow rate is equal to inlet flow
rate.
6. 20ml of product was collected and transferred into the flask containing 20 ml of standardized
hydrochloric acid for arresting the reaction.
7. This solution was mixed thoroughly and titrated against standardized NaOH.
8. The titrate value was repeated for different flow rate and result were tabulated.
OBSERVATION:
Normality of ethyl acetate, N4 = 0.1 N
Normality of acetic acid, N1 = 0.1 N
Diameter of reactor, d = 15 cm
Length of reactor, L = 25 cm

TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)

BURETTE READING OF NaOH


VOLUME OF ACETIC CONCORDANT
S.NO (ml)
ACID VALUE (ml)
(ml) Initial Final

Volume of acetic acid, V1 = 20 ml


Normality of acetic acid, N1 = 0.1N
Volume of NaOH, V2 = ml
Normality of NaOH, N2 = ?
V1N1 = V2N2
N2 = V1N1/ V2
N2 = --------------------- N.
TABULATION II:
Standardization of Hcl:
Burette solution- NaOH
Pipette solution- Hcl
(20ml)

BURETTE READING of NaOH CONCORDANT


S.NO VOLUME OF Hcl (ml) (ml) VALUE (ml)
Initial Final

Volume of NaOH, V2 = -------------- ml


Normality of NaOH, N2 = --------------N

Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:

Volume of
Volume of
Volumetric Volumetric Volume of Volume of Hcl not
Hcl used to
flow rate of flow rate of reaction Hcl added in used to
S.NO arrest the
NaOH ethyl acetate mixture the conical arrest the
reaction
(LPM) (LPM) collected (ml) flask (V0, ml) reaction
(V6, ml)
(V4, ml)

TABULATION IV:

Titre value of
Space time,
NaOH, CA, (mole/lit) XA (no unit) XA/ (1- XA) XA/ (1- XA)2
(Ʈ, sec)
(V5, ml)
CALCULATION:

Initial concentration of NaOH, CA0 = (N2 X Vol. flow rate of NaOH) / Total vol. flow rate

CA0 =

CA0 = ___ _ _ _ _ mole/lit.

Initial concentration of EA, CB0 = (N4 X Vol. flow rate of EA) / Total vol. flow rate

CB0 =

CB0 = ___ _ _ _ __ mole/lit.

CA0 = CB0 (Since equimolar)

Volume of Hcl not used for


arresting the reaction, V4 = (V5 X N2) / N3

V4 = ___ _ _

Volume of Hcl used for


arresting the reaction, V6 = V0 – V4
V6 =
V6 = ___ _ __

Moles of Hcl used for arresting = V6 X N3


=
= ____________ moles.
Moles of Hcl used for arresting = Moles of unreacted NaOH in the conical flask.

Concentration of NaOH in the


conical flask, CA = Moles of unreacted NaOH / (Volume of NaOH in
the reaction mixture)
CA =
CA = ___ _ _
Conversion, XA = (CA0 – CA) / CA0

XA =

XA / (1- XA)2 = ___ _ _ _ _

Space time, Ʈ = Volume of reactor / Total vol. flow rate


Volume of reactor, V = πr2L
=
V = ___ _ __

Ʈ =
Ʈ = ___ _ _ _.

Plot the graph between XA / (1- XA)2 in y axis and Ʈ in x axis.

Determine slope k CA0


Find k from the slope value.
RESULT:
Thus the kinetic studies for saponification reaction of equimolar quantities of ethyl acetate and NaOH
is prepared and the rate constant is determined to be k =
EXP NO.
DATE:
Kinetic studies CSTR in series
Aim:

To determine the rate constant and kinetis for saponification of equimolar quantity of ethyl acetate
andsodium hydroxide in a CSTR

Apparatus Required:
Cascade CSTR setup (series)
Conical flask
Beaker
Standard measuring flask
Measuring jar
Stop watch
Chemicals Required:
Sodium hydroxide (NaOH)
Ethyl acetate (CH3COOC2H5)
Acetic acid (CH3COOH)
Water (H2O)
Hydrochloric acid (Hcl)
Phenolphthalein indicator
Theory:
Consider a system of mixed flow reactor (or) CSTR connected in series. Though the concentration is
uniform ineach reactor, there is, nevertheless a change in concentration as the fluid moves from reactor to
reactor. This stepwise drop in the concentration suggests that the large, the number of units in series, the
closer should be the behaviour of the system, approaches plug flow. The reaction between sodium hydroxide
and ethyl acetate is represented by the stoichiometry as follows:

NaOH +CH3COOC2H5 gives CH3COONa + C2H5OH

The design equation for MFR is,


kƮCA0 = XA / (1- XA)2
Procedure:
1. The solution of sodium hydroxide, hydrochloric acid, acetic acid and ethylacetate of
required strength are prepared.
2. Sodium hydroxide and hydrochloric acid solutions are standardized.
3. The storage reservoirs were filled with -------------- lit of sodium hydroxide
and ---------- lit of ethyl acetate solution.
4. The required flow rates of sodium hydroxide and ethyl acetate were adjusted using rotameter
such that the flow rate of both sodium hydroxide and ethyl acetate were same (for feeding
on equimolar quantity of sodium hydroxide and ethyl acetate).
5. Steady state conditions were allowed to be obtained. i.e. outlet flow rate isequal to inlet flow
rate.
6. 20ml of product was collected from each reactor and transferred into the flask containing 20
ml of standardized hydrochloric acid for arresting the reaction.
7. This solution was mixed thoroughly and titrated against standardized NaOH.
8. The titrate value was repeated for different flow rate and result were tabulated.
OBSERVATION:
Normality of ethyl acetate, N4 = 0.1N
Normality of acetic acid, N1 = 0.1N
Diameter of reactor, d = cm
Length of reactor, L = cm

TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)

BURETTE READING OF NaOH (ml)


VOLUME OF ACETIC ACID CONCORDANT
S.NO
(ml) VALUE (ml)
Initial Final

Volume of acetic acid, V1 = 20 ml


Normality of acetic acid, N1 = 0.1N
Volume of NaOH, V2 = ml
Normality of NaOH, N2 = ?
V1N1 = V2N2
N2 = V1N1/ V2
N2 = --------------------- N.
TABULATION II:
Standardization of Hcl:
Burette solution- NaOH
Pipette solution- Hcl
(20ml)

BURETTE READING of NaOH (ml) CONCORDANT


S.NO VOLUME OF Hcl (ml)
VALUE (ml)
Initial Final

Volume of NaOH, V2 = -------------- ml


Normality of NaOH, N2 = --------------N

Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:

For Flow rate 1:

Volume of Volume of Volume of Hcl


Volumetric Volumetric Volume of Hcl
reaction Hcl added in not used to
flow rate of flow rate of used to arrest
Reactor mixture the conical arrest the
NaOH ethyl acetate the reaction
collected flask reaction
(LPM) (LPM) (V6, ml)
(ml) (V0, ml) (V4, ml)

TABULATION IV:

Titre value of
Space time,
NaOH, CA, (mole/lit) XA (no unit) XA/ (1- XA) XA/ (1- XA)2
(Ʈ, sec)
(V5, ml)
TABULATION V:

For Flow rate 2:

Volume of
Volume of Volume of Hcl
Volumetric Volumetric Volume of Hcl Hcl used
reaction not used to
flow rate of flow rate of added in the to arrest
Reactor mixture arrest the
NaOH ethyl acetate conical flask the
collected reaction
(LPM) (LPM) (V0, ml) reaction
(ml) (V4, ml)
(V6, ml)

TABULATION VI:

Titre value of
Space time,
NaOH, CA, (mole/lit) XA (no unit) XA/ (1- XA) XA/ (1- XA)2
(Ʈ, sec)
(V5, ml)
CALCULATION:

Initial concentration of NaOH, CA0 = (N2 X Vol. flow rate of NaOH) / Total vol. flow rate

CA0 =

CA0 = ___ _ _ _ _ mole/lit.

Initial concentration of EA, CB0 = (N4 X Vol. flow rate of EA) / Total vol. flow rate

CB0 =

CB0 = ___ _ _ _ __ mole/lit.

CA0 = CB0 (Since equimolar)

Volume of Hcl not used for


arresting the reaction, V4 = (V5 X N2) / N3

V4 = ___ _ _

Volume of Hcl used for


arresting the reaction, V6 = V0 – V4
V6 =
V6 = ___ _ __

Moles of Hcl used for arresting = V6 X N3


=
= ____________ moles.
Moles of Hcl used for arresting = Moles of unreacted NaOH in the conical flask.

Concentration of NaOH in the


conical flask, CA = Moles of unreacted NaOH / (Volume of NaOH in
the reaction mixture)
CA =
CA = ___ _ _ __
Conversion, XA = (CA0 – CA) / CA0
XA = ___ _ _ __

XA / (1- XA) = = ___ _ _ _ __

XA / (1- XA)2 = ___ _ _ _ _

Space time, Ʈ = Volume of reactor / Total vol. flow rateVolume of reactor,

V = πr2L

V = ___ _ __

Ʈ = ___________ _.

Plot the graph between XA / (1- XA)2 in y axis and Ʈ in x axis.

Determine slope kCA0


Find k from the slope value.
RESULT:
Thus the kinetic studies for saponification reaction of equimolar quantities of ethyl acetate and
NaOH is performed and the percentage conversion for different flow rates have beencalculated and the
rate constant is determined.
K=
% conversion
Flow rate
Reactor 1 Reactor 2 Reactor 3
EXP NO.
DATE:
Kinetic studies in MFR followed by PFR
Aim:

To determine the intermediate conversion and overall conversion in MFR followed by


PFR
Apparatus Required:
CSTR setup
PFR setup
Conical
flaskBeaker
Standard measuring
flaskMeasuring jar
Stop watch
Chemicals Required:
Sodium hydroxide (NaOH)
Ethyl acetate
(CH3COOC2H5)Acetic acid
(CH3COOH) Water (H2O)
Hydrochloric acid (Hcl)
Phenolphthalein
indicator
Theory:
A mixed flow reactor or a CSTR is operated at steady state. There is no accumulation. The total
mass flow rate at which the reactants are fed to the reactor is equal to the mass flow rate at which the
products are withdrawn from the reactor. Therefore the properties in the CSTR do not change with time.
The concentration of reactants drops to the outlet concentration immediately on entering the CSTR. The
concentration of the material does not vary with time. Since the reactor is well mixed, the concentration
throughout the reactors is uniform i.e. there is no spacial variation in concentration in the reactors at any
time. Thus the rate of reaction in a CSTR is constant throughout the reactor at fixed temperature where
as in a PFR.

The PFR is operated at steady state i.e. the conditions in the plug flow reactor do not vary with time.
The steady state flow condition means that the total mass
flow rate at which the reactants are fed to the reactor is equal to the total mass flow rate of the products
withdrawn from the reactors. There is no accumulation in the plug flow reactor. The concentration varies
in the axial direction. Therefore there is a concentration gradient along the axial direction (there is no
mixing along axial direction) but there may be mixing in the radial direction. Therefore a plug flow
reactor is otherwise called as an ideal tubular reactor.

The reaction between sodium hydroxide and ethyl acetate can be represented as,

NaOH + CH3COOC2H5  CH3COONa + C2H5OH


The design equation for MFR is,

kƮCA0 = XA / (1- XA)2

The design equation for PFR is,

kƮCA0 = XA / (1- XA)

Procedure:
1. The solution of sodium hydroxide, hydrochloric acid, acetic acid and ethylacetate of
required strength are prepared.
2. Sodium hydroxide and hydrochloric acid solutions are standardized.
3. The storage reservoirs were filled with --------- lit of sodium hydroxide and
------------- lit of ethyl acetate solution.
4. The required flow rates of sodium hydroxide and ethyl acetate were adjusted using rotameter
such that the flow rate of both sodium hydroxide and ethyl acetate were different (for feeding
on non equimolar quantity of sodium hydroxide and ethyl acetate).
5. Steady state conditions were allowed to be obtained. i.e. outlet flow rate is equal to inlet flow
rate.
6. 20ml of product was collected from CSTR and transferred into the flask containing 20 ml
of standardized hydrochloric acid for arresting the reaction.
7. This solution was mixed thoroughly and titrated against standardized NaOH.
8. 20ml of product was collected from PFR and transferred into the flask containing 20 ml of
standardized hydrochloric acid for arresting the reaction
9. This solution was mixed thoroughly and titrated against standardized NaOH.
10. The titrate value was repeated for different flow rate and result were tabulated.
OBSERVATION:
Normality of ethyl acetate, N4 = 0.1N
Normality of acetic acid, N1 = 0.1N
Diameter of reactor, d = cm
Length of reactor, L = cm

TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)

BURETTE READING OF NaOH (ml)


VOLUME OF ACETIC ACID CONCORDANT
S.NO
(ml) VALUE (ml)
Initial Final

Volume of acetic acid, V1 = 20 ml


Normality of acetic acid, N1 = 0.1N
Volume of NaOH, V2 = ml
Normality of NaOH, N2 = ?
V1N1 = V2N2
N2 = V1N1/ V2
N2 = --------------------- N.
TABULATION II:
Standardization of Hcl:
Burette solution- NaOH
Pipette solution- Hcl
(20ml)

BURETTE READING of NaOH (ml) CONCORDANT


S.NO VOLUME OF Hcl (ml)
VALUE (ml)
Initial Final

Volume of NaOH, V2 = -------------- ml


Normality of NaOH, N2 = --------------N

Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:

Flow rate Titre value Concentration CA Concentration CB


Conversion
(LPM) (ml) (mole/lit) (mole/lit)

S.No Inter
MFR+ MFR+ MFR+ Over
NaOH EA MFR MFR MFR media
PFR PFR PFR all
te
CALCULATION:
MFR: PFR:
Diameter of MFR = Diameter of PFR =
Length of MFR = Length of PFR =
Volume of reactor = πr2L Volume of reactor = πr2L

= =

Concentration of NaOH in the feed stream, CA0 = (StrengthxFlow rate of NaOH)/ Total flow
rateCA0 =

Concentration of EA in the feed stream, CB0 = (StrengthxFlow rate of EA)/ Total flow rate
CB0 =

CA, Intermediate = [(NHcl x VHcl) – (NNaOH x VNaOH)]MFR / Total vol of sample in the conical
flaskCA, Intermediate =

CB, Intermediate = CA0 – CB0 + CA,


IntermediateCB, Intermediate =

CA, Overall = [(NHcl x VHcl) – (NNaOH x VNaOH)]MFR + PFR / Total vol of sample in the conical flask
CA, Overall =
CA, Overall =

Intermediate conversion, XA = (CA0 - CA, Intermediate)/ CA0


XA =

Overall conversion, XA =
XA =
RESULT:
The conversion for the combined system of MFR-PFR is studied for different flow rates
and the results are given as follows:

Flow rate (LPM) Conversion%

NaOH Ethyl Acetate Intermediate Overall


EXP NO.
DATE:
Effect of temperature on reaction rate constant and conversion
Aim:

To determine the effect of temperature on the reaction rate constant, k and determine the
activation energy E for the saponification reaction.
Apparatus Required:
MFR setup
Conical flask
Beaker
Standard measuring flask
Measuring jar
Stop watch
Heater
Chemicals Required:
Sodium hydroxide (NaOH)
Ethyl acetate (CH3COOC2H5)
Acetic acid (CH3COOH)
Water (H2O)
Hydrochloric acid (Hcl)
Phenolphthalein indicator
Theory:
In an ideal plug flow reactor (PFR) there is no mixing in the direction of flow and complete
mixing perpendicular to the direction of flow. Concentration of the reactant varies along the length of
the reactor but not in the radial direction. V is the volume of the reactor, Vo is the volumetric feed rate,
CAo is the feed conc. of A, x is the degree of conversion. In case of a Coil, turbulence is introduced due
to frequent change in direction of flow and presence of secondary flow. So a higher value of k is expected
in case of a coil type PFR. For steady state rate operation of a PFR: In case of a Coil, turbulence is
introduced due to frequent change in direction of flow and presence of secondary flow. So a higher value
of k is expected in case of a coil type PFR.
Procedure:
1. Fill the tanks with sodium hydroxide and ethyl acetate solution.
2. Fill the water bath with water.
3. Start the heater and stirrer of the bath.
4. Using rotameter set the different flow rate for both the solution i.e. CA0 not equal to CB0
5. After steady state is achieved, collect 20 ml of the sample of the liquid at the outlet in
theconical flask which already contains 20 ml of Hcl
6. Using phenolphthalein as indicator, titre this solution against NaOH
7. Collect the sample for every 5 degree rise in temperature and repeat the steps.
OBSERVATION:
Normality of ethyl acetate, N4 = 0.1N
Normality of acetic acid, N1 = 0.1N
Diameter of reactor, d = cm
Length of reactor, L = cm

TABULATION I:
Standardization of NaOH:
Burette solution- NaOH
Pipette solution- Acetic acid (20ml)

BURETTE READING NaOH (ml)


VOLUME OF ACETIC ACID CONCORDANT
S.NO
(ml) VALUE (ml)
Initial Final

Volume of acetic acid, V1 = 20 ml


Normality of acetic acid, N1 = 0.1N
Volume of NaOH, V2 = ml
Normality of NaOH, N2 = ?
V1N1 = V2N2
N2 = V1N1/ V2
N2 = --------------------- N.
TABULATION II:
Standardization of Hcl:
Burette solution- NaOH
Pipette solution- Hcl
(20ml)

BURETTE READING of NaOH (ml) CONCORDANT


S.NO VOLUME OF Hcl (ml)
VALUE (ml)
Initial Final

Volume of NaOH, V2 = -------------- ml


Normality of NaOH, N2 = --------------N

Volume of Hcl, V3 = 20 ml
Normality of Hcl, N3 = ?
V2N2 = V3N3
N3 = V2N2/ V3
N3 = --------------------- N.
TABULATION III:

Vol. of
NaoH
Temp CA CB k -r
S. (Titre
%Conversion
No value)

0c
gmole Integ Differ Differe
ml gmole Integral
/lit /lit ral ential ntial

AVERAGE VALUE
CALCULATION:
Concentration of NaOH in the feed stream, CA0 = (Strength x Flow rate of NaOH)/ Total flow
rateCA0 =

Concentration of EA in the feed stream, CB0 = (Strength x Flow rate of EA)/ Total flow rate
CB0 =

CA = [(NHcl x VHcl) – (NNaOH x VNaOH)] / Total vol of sample in the conical flask
CA =

CB = CA0 – CB0 +
CA CB =

-r (Differential) = (CA0 – CA) / (tf – t0)


tf = final time
t0 = Initial time
-r =
XA = (CA0 - CA) /
CA0XA =
k = (1/tCA0) ( XA – (1- XA))
[Integral]k = -r (integral)
Assuming CA = CB

-r (integral) = k C2 A
-r (integral) =

Activation energy:
ln (r2 / r1) = -E/R (1/ T1 – 1/T2)
Integral: E =
=
Differential: E =
E=
RESULT:
The value of rate constant for reaction between NaOH and EA is,
Kdifferential =
Kintegral =
The activation energy is determined as,

ACTIVATION ENERGY ACTIVATION ENERGY


TEMPERATURE (k)
(Integral) (Differential)
EXP NO.
DATE:
RTD Studies in MFR
Aim: To study the residence time distribution in a CSTR.
Chemicals required:
 Concentrated sulphuric acid
 NaOH
 Phenolphthalein indicator
Apparatus Required:
CSTR Setup
Theory:
Plug and mixed flow are the two extreme flow behavior of through reactors, these twoflow
behaviors are said to be ideal. In the ideal batch reactors all the atoms of the material withinreactor for a
identical length of time. The time in which the atoms spent is called the residence time of atom in
reactor. The ideal plug flow and batch reactors are the only two classes ofreactors in which all the
atoms have spent same residence time. In all the other types inside the reactor there is a distribution of
residence time of the material within the reactor.
Consider a CSTR, feed introduced in CSTR at any given time becomes completely mixed with
the materials already in the reactor. In other words, some of the atoms entering into the CSTR leave it
almost immediately because the material is being continuously withdrawn from reactor, other atoms
remain in the reactor almost forever because all the material is never removed from the reactor at one
time. Many of the atoms leave the reactor after spending a period of time somewhere in the vicinity of
mean residence time. In any reactor the distribution of the residence time can significantly affect its
performance in the residence time distribution of reactor is a characteristic of mixing that occurs in
reactor.
The RTD can be measured by injecting an inert chemical material called tracer, into reactor at
t=0 and measuring the tracer concentration, C in the effluent stream as function of time.The two most
used methods of injecting tracer are pulse, step input. The effluent concentration versus time is referred
to as C curve in RTD analysis with no tracer initially present anywhere imposes a step input of tracer
concentration C0 on the fluid stream entering the vessel. Then a time record of a tracer in the exit
stream from the vessel measured as C/Co is called F curve. For a closed vessel.
Procedure:
1. Water is fed into the reactor at constant flow rate.
2. The system is allowed to reach steady state, (i.e) outlet flow rate is equal to inlet flow rate.
3. After steady state is reached, concentrated sulphuric acid solution is injected as a tracer bymeans
of syringe into the reactor.
4. The stopwatch is started simultaneously and the sample is collected for 0th minute.
5. The 20ml of sample are collected at regular intervals of 3 minutes from the outlet stream indifferent
beakers.
6. The sample were transformed to conical flask and titrated against N NaOH with
phenolphthalein as an indicator.
7. The concentration of H2SO4 from the samples was determined from the burette reading.
8. The F and E curves were plotted.
9. Thus the experiment of RTD in CSTR was performed and the readings were tabulated and curves
were plotted successfully.
Observation:

Flow rate of water =

Normality of NaOH =

Tabulation:

Volume of
Volume of NaOH required Concentration
Time
S.No sample collected, for neutralizing of H2SO4 in C/C0
(min)
V1 (ml) the sample, V2 sample, N1
(ml)
Model calculations:

Concentration of H2SO4 in the sample, N1 = (V2 N2)/ V1 =

N1 =

C / C0 = N1 / N2 =

GRAPH1: Plot the graph between C/C0 (y axis) time (x axis) and identify five different slope
values.

Time (min)

Slope (min-1)

GRAPH 2: Plot the graph between slope which was identified from graph 1 (y axis) time (x
axis).
RESULT:

Thus the experiment of RTD in CSTR was performed and the reading was tabulated and
curve was plotted successfully.

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