Laboratory Man

FACULTY OF ENGINEERING AND TECHNOLOGY

DIPLOMA STUDIES
CHEMICAL REACTION ENGINEERING LAB

(03602360)
6th SEMESTER
CHEMICAL ENGINEERING DEPARTMENT

Laboratory Manual

DEPARTMENT OF CHEMICAL ENGINEERING

PARUL INSTITUTE OF TECHNOLOGY-DIPLOMA STUDIES
PARUL UNIVERSITY,WAGHODIA VADODARA
 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

PREFACE
The Chemical Reaction Engineering Course at PARUL UNIVERSITY,
WAGHODIA, VADODARAare designed in such a way that students develop the basic
understanding of the subject in the theory classes and then try their hands on the experiments
to realize the various physical phenomena learnt during the theoretical sessions. The main
objective of the Chemical Reaction Engineering laboratory course is: Learning Reaction of
kinetics through Experimentations. All the experiments are designed to illustrate various
phenomena in different areas of Chemical process and also to expose the students to various
instruments and their uses.

The objective of this Chemical Reaction Engineering Is to provide a comprehensive

source for all the experiments included in the Chemical Reaction Engg laboratory course. It
explains all the aspects related to every experiment such as: basic underlying physical
principle, details of the instruments, how to use these instruments for the desired purpose, the
theoretical formalism & formulae, procedure of performing the experiment and how to
calculate the desired results from the observations etc. It also gives sufficient information on
how to interpret and discuss the obtained results.

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Instructions to students

1. The main objective of the Chemical Reaction Engineering laboratory is: Learning
Chemical Reaction Engineering through Experimentation. All the experiments are
designed to illustrate various phenomena in different areas of Chemical Reaction
Engineering and also to expose the students to various instruments and their uses.
2. Be prompt in arriving at the laboratory and always come well prepared for the
experiment.
3. Be careful while working on the equipment operated with high voltage power supply.
4. Work quietly and carefully. Give equal opportunity to all your fellow students to work on
the instruments.
5. Every student should have his/her individual copy of the Chemical Reaction
Engineering-I Practical Book.
6. Every student have to prepare the notebooks specifically reserved for the Chemical
Reaction Engineering practical work: Chemical Reaction Engineering Practical Book”
7. Every student has to necessarily bring his/her Chemical Reaction Engineering Practical
Book, Chemical Reaction Engineering Practical Class Notebook and Chemical Reaction
Engineering-I Practical Final Notebook, when he/she comes to the Practical to perform
the experiment.
8. Record your observations honestly. Never makeup reading or doctor them either to get a
better fit on the graph or to produce the correct result. Display all your observations on
the graph (if applicable)
9. All the observations have to be neatly recorded in the Chemical Reaction Engineering
Practical Class Notebook (as explained in the Chemical Reaction Engineering Practical
Book) and verified by the instructor before leaving the laboratory.
10. If some of the readings appear to be wrong then repeat the set of observations carefully.
11. Do not share your readings with your fellow student. Every student has to produce his/her
own set of readings by performing the experiment separately.
12. After verification of the recorded observations, do the calculation in the Chemical
Reaction Engineering Practical Class Notebook (as explained in the Chemical Reaction
Engineering Practical Book) and produce the desired results and get them verified by the
instructor.
13. Never forget to mention the units of the observed quantities in the observation table. After
calculations, represent the results with appropriate units.
14. Calculate the percentage error in the results obtained by you if the standard results are
available and also try to point out the sources of errors in the experiment.
15. Find the answers of all the questions mentioned under the section ‘Find the Answers’ at
the end of each experiment in the Chemical Reaction Engineering Practical Book.
16. Finally record the verified observations along with the calculation and results in the
Chemical Reaction Engineering Practical Notebook.
17. Do not forget to get the information of your next allotment (the experiment which is to be
performed by you in the next laboratory session) before leaving the laboratory from the
Technical Assistant.
18. The grades for the Chemical Reaction Engineering practical course work will be awarded
based on your performance in the laboratory, regularity, recording of experiments in the
Chemical Reaction Engineering Practical Final Notebook, lab quiz, regular viva-voce
and end-term examination.

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

CERTIFICATE
This is to certify that

Mr./Ms.…………………………………………………

with enrolment no. …………………………has successfully

completed his/her experiments

In the Chemical Reaction Engineering laboratory (03602360)

during the academic year…………

Date:

Signature of faculty: Signature of HOD:

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

INDEX

Date of Date of Sign

SR. Page No Performance Assessment Marks
NO Title out of
. 10
From To
Overview of Chemical
1)
Reaction Engineering
The Kinetics Of the
2) Reaction & Order Of
Reaction
Determination
3)
Activation Energy

4) Determination of
Frequency Factor
Kinetic Studies in a
5) Continuous Stirred Tank
Reactor

Pseudo-First Order
6) Kinetics

Differential Method of
7) Analysis

Integral Method of
8) Analysis

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-1

Overview of Chemical Reaction Engineering

● Every industrial chemical process is designed to produce economically a desired

product from a variety of starting materials through a succession of treatment steps.
Figure shows a typical situation.

● The raw materials undergo a number of physical treatment steps to put them in the
form in which they can be reacted chemically. Then they pass through the reactor. The
products of the reaction must then undergo further physical treatment-separations,
purifications, etc. for the final desired product to be obtained.

● Design of the reactor is no routine matter, and many alternatives can be proposed for a
process. In searching for the optimum it is not just the cost of the reactor that must be
minimized. One design may have low reactor cost, but the materials leaving the unit
may be such that their treatment requires a much higher cost than alternative designs.
Hence, the economics of the overall process must be considered.

1 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Much of this subject deals with finding the expression to relate input to output for various
Kinetics and various contacting patterns,
or
Output = f [input, kinetics, contacting]

A chemical species is said to have reacted when it has lost its chemical identity. There are
three ways for a species to lose its identity:

1. Decomposition CH3CH3🡪 H2 + H2C=CH2

2. Combination N2 + O2🡪 2 NO
3. Isomerization C2H5CH=CH2🡪 CH2=C(CH3)2

• The reaction rate is the rate at which a species loses its chemical identity per unit
volume.
• The rate of a reaction (mol/dm3/s) can be expressed as either
• The rate of Disappearance: -rAor

• The rate of Formation (Generation): rA

• Consider the isomerization

• A🡪B

• rA = the rate of formation of species A per unit volume

• -rA = the rate of a disappearance of species A per unit volume

• rB = the rate of formation of species B per unit volume

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Reaction Mass Balance:

3 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-2

The Kinetics of the Reaction & Order of Reaction

OBJECTIVE:

To determine the order of reaction (n) and the reaction rate constant (k) for the given
saponification reaction of ethyl acetate in aqueous sodium hydroxide solution.
APPARATUS:

● Batch reactor with agitator and temperature batch.

● Pipette.
● Burette.
● Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

● 0.05 N Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

● 0.05 N Sodium hydroxide solution
● 0.05 N HCl solution
● Phenolphthalein as indicator etc.

THEORY:

Saponification of ethyl acetate proceeds as follows:

C H 3 COO C 2 H 5 + NaOH → C H 3 COO Na + C 2 H 5 O H

(A) + (B) → Products

The reaction in the reversible direction can be neglected under the specific conditions i.e. the
excess of NaOH.

Working Rate Equation:

− rA=− dCA = k2 CA CB = k2 CA0 2 (1 − XA) (M − XA), where M = CB0/dtC A0

4 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

PROCEDURE:

● Prepare 0.05 N 300 ml ethyl acetate and 0.05 N 300 ml NaOH.

● Prepare a solution of 0.05 N 100 ml HCl and 0.05 N 100 ml NaOH solutions for the
titration.

● Use phenolphthalein as an indicator.

● Take 6 Nos. of 250 ml conical flasks and put 10 ml of 0.05 N HCl in each flask.

● Take 0.05 N NaOH solution in the burette.

● Adjust the temperature of the water bath at 40 oC.

● Take 300 ml each of 0.05 N CH3COOC2H5 and 0.05 N NaOH in two separate flasks
and keep these in the water bath for about 15 min to preheat the solutions.

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

● Transfer these solutions quickly in the batch reactor. Start immediately the mixer and
the stopwatch.

● At regular intervals of 15 min., withdraw 10 ml of reaction mixture and put it in the

conical flask containing 0.05 N HCl. Take at least 6 samples at regular intervals of
time.

● Titrate the excess 0.05 N HCl in each flask using 0.05 N NaOH from burette and
phenolphthalein as indicator.

OBSERVATION & OBSERVATION TABLE:

● Reaction temp = oC = K
● Conc. of HCl = N1 = 0.05 N
● Conc. of NaOH (A)= N3 = 0.05 N
● Conc. of Ethyl acetate (B) = 0.05 N
● Vol. of Ethyl acetate taken = 300 ml
● Vol. of Sodium hydroxide = 300 ml
● Initial Conc. of NaOH (A) in the mixture, CAO = 0.05 N (g mole/L)
● Initial Conc. of Ethyl acetate (B) in the mixture, CBO = 0.05 N (g mole/L)

Sr. Time Volume of HCL Volume of sample for Volume of NaOH

No. (min.) used, V1 ml titration, V2 ml for Titration, V 3 ml
1 15
2 30
3 45
4 60
5 75

CALCULATIONS:.

Estimation of un-reached NaOH in the reaction mixture (CA)

Volume of 0.05 N HCl taken in conical flask V1= 20 ml

Volume of reaction mixture sample added V2 = 10 ml
Volume of 0.05 N NaOH used in titration for neutralization of excess 0.05 N HCl,
V3 NaOH = ml

6 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Reaction between NaOH and HCl is:

NaOH + HCl —> NaCl + H2O

i.e., 1 mole of NaOH reacts with 1 mole of HCl

No. of moles 0.05 N HCl present initially in conical flask = N1V1=0.05 x V1 x 10-3 g moles

No. of moles of 0.05 N NaOH used (No. of moles of 0.05 N HCl unreacted) = N3V3
= N3 x V3 NaOH x 10-3 g moles
= 5 x 10-5 x V3 NaOH

No. of moles of HCl reacted with excess moles of NaOH in the reaction mixture
(No. of moles of NaOH unreacted in the reaction mixture)
NA = (0.05 x V1 x 10-3 - 5 x 10-5 x V3 NaOH) g moles

Concentration of unreacted NaOH in the reaction mixture CA= NA /V2

RESULTS AND DISCUSSIONS:

Sr. No. Time (Min.) Experimental Concentration(CA)

1 15
2 30
3 45
4 60
5 75
GRAPHS:

(1) Plot experimental and theoretical conversion versus time.

7 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

INTIGRAL METHOD OF ANALYSIS

Plot Inverse con versus time t, yield straight line confirm second order kinetics and slope will

Gives rate constant k2 = -------- lit. / Mol min at room temperature _______0C.

8 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-3

Determination of Activation Energy

OBJECTIVE:

To determine activation energy of saponification reaction between ethyl acetate and sodium
hydroxide.

k2 = k 0exp (- E /RT), Take k 2 = 6.5 liter / g mol min at 25 0C.

.
APPARATUS:

1. Batch reactor with agitator and temperature batch.

2. Pipette.
3. Burette.
4. Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

1. 0.05 N Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

2. 0.05 N Sodium hydroxide solution
3. 0.05 N HCl solution
4. 0.05 N oxalic acid solution (3.15 gm per liter of solution)
5. Phenolphthalein as indicator etc.

THEORY:

● Saponification of ethyl acetate proceeds as follows:

● C H 3 COO C 2 H 5 + NaOH → C H 3 COO Na + C 2 H 5 O H
● (A) (B) → Products
● The reaction in the reversible direction can be neglected under the specific conditions
i.e. the excess of NaOH.

9 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

PROCEDURE:

(1) At room temperature:

● Pour 10 ml of 0.05 N HCl to each of the ten 250 ml conical flasks and mark them.
● Pour 300 ml of 0.05 N acetate solutions to the reactor.
● Start the stirrer and record the temperature (T1). Pour 300 ml of 0.05 N NaOH
solutions to the reactor vessel as quickly as possible.
● Immediately start the stopwatch and draw a 10 ml sample from the reactor at a regular
time interval of one minute. Pour this sample into the labeled conical flasks.
● Titrate the excess HCL with standard NaOH (0.05 N) solution.

(2) At temperature T1 + 10 0C, T1 + 20 0C and T1 + 30 0C:

● Preliminary preparations for this test run will be the same as in the case of the
previous one.
● Temperature of the ethyl acetate in the reactor is brought to T1 + 10 0C by starting
circulating the hot water to the jacket while the stirrer is kept on. 300 ml of 0.05 N
NaOH solution is taken in a beaker or flask and brought to temperature T1 + 10 0C in
a mantle heater.
● These two warm solutions are brought in contact by pouring the NaOH solution to the
reactor.
● The samples are carried out at a regular time interval for finding the progress of the
reaction.
● Follow the same procedure for the other two temperatures.

OBSERVATION TABLE:

●
Sr. Time (min.) Volume of NaOH required to titrate the excess acid, V3 ml
No.
T10C T1 + 10 0C T1 + 20 0C T1 + 30 0C
1
2
3
4
5

CALCULATIONS:.

Estimation of un-reached NaOH in the reaction mixture (CA)

10 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Volume of 0.05 N HCl taken in conical flask V1= 20 ml

Volume of reaction mixture sample added V2 = 10 ml
Volume of 0.05 N NaOH used in titration for neutralization of excess 0.05 N HCl,
V3 NaOH = ml

Reaction between NaOH and HCl is:

NaOH + HCl —> NaCl + H2O

i.e., 1 mole of NaOH reacts with 1 mole of HCl

No. of moles 0.05 N HCl present initially in conical flask = N1V1=0.05 x V1 x 10-3 g moles

No. of moles of 0.05 N NaOH used (No. of moles of 0.05 N HCl unreacted) = N3V3
= N3 x V3 NaOH x 10-3 g moles
= 5 x 10-5 x V3 NaOH

No. of moles of HCl reacted with excess moles of NaOH in the reaction mixture
(No. of moles of NaOH unreacted in the reaction mixture)
NA = (0.05 x V1 x 10-3 - 5 x 10-5 x V3 NaOH) g moles

Concentration of unreacted NaOH in the reaction mixture CA= NA /V2

RESULTS AND DISCUSSIONS:

Sr. No. Time (Min.) Experimental Concentration(CA)

1 15
2 30
3 45
4 60
5 75
GRAPHS:

(2) Plot experimental and theoretical conversion versus time.

11 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-4

Determination of Frequency Factor

OBJECTIVE:

To verify the Arrhenius Plot for saponification of Ester with NaOH and to determine
the Frequency Factor of this reaction.
k2 = k 0exp (- E /RT), Take k 2 = 6.5 liter / g mol min at 25 0C.
.
APPARATUS:

1. Batch reactor with agitator and temperature batch.

2. Pipette.
3. Burette.
4. Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

1. 0.05 N Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

2. 0.05 N Sodium hydroxide solution
3. 0.05 N HCl solution
4. 0.05 N oxalic acid solution (3.15 gm per liter of solution)
5. Phenolphthalein as indicator etc.

THEORY:

Saponification of ethyl acetate proceeds as follows:

C H 3 COO C 2 H 5 + NaOH→ C H 3 COO Na + C 2 H 5 O H

(A) (B) → Products
The reaction in the reversible direction can be neglected under the specific conditions i.e. the
excess of NaOH.

PROCEDURE:

(3) At room temperature:

● Pour 10 ml of 0.05 N HCl to each of the ten 250 ml conical flasks and mark them.
● Pour 300 ml of 0.05 N acetate solutions to the reactor.

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

● Start the stirrer and record the temperature (T1). Pour 300 ml of 0.05 N NaOH
solutions to the reactor vessel as quickly as possible.
● Immediately start the stopwatch and draw a 10 ml sample from the reactor at a regular
time interval of one minute. Pour this sample into the labeled conical flasks.
● Titrate the excess HCL with standard NaOH (0.05 N) solution.

(4) At temperature T1 + 10 0C, T1 + 20 0C and T1 + 30 0C:

● Preliminary preparations for this test run will be the same as in the case of the
previous one.
● Temperature of the ethyl acetate in the reactor is brought to T1 + 10 0C by starting
circulating the hot water to the jacket while the stirrer is kept on. 300 ml of 0.05 N
NaOH solution is taken in a beaker or flask and brought to temperature T1 + 10 0C in
a mantle heater.
● These two warm solutions are brought in contact by pouring the NaOH solution to the
reactor.
● The samples are carried out at a regular time interval for finding the progress of the
reaction.
● Follow the same procedure for the other two temperatures.

OBSERVATION TABLE:

●
Sr. Time (min.) Volume of NaOH required to titrate the excess acid, V3 ml
No.
T10C T1 + 10 0C T1 + 20 0C T1 + 30 0C
1
2
3
4
5

CALCULATIONS:.

Estimation of un-reached NaOH in the reaction mixture (CA)

Volume of 0.05 N HCl taken in conical flask V1= 20 ml

Volume of reaction mixture sample added V2 = 10 ml
Volume of 0.05 N NaOH used in titration for neutralization of excess 0.05 N HCl,
V3 NaOH = ml

Reaction between NaOH and HCl is:

NaOH + HCl —> NaCl + H2O

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

i.e., 1 mole of NaOH reacts with 1 mole of HCl

No. of moles 0.05 N HCl present initially in conical flask = N1V1=0.05 x V1 x 10-3 g moles

No. of moles of 0.05 N NaOH used (No. of moles of 0.05 N HCl unreacted) = N3V3
= N3 x V3 NaOH x 10-3 g moles
= 5 x 10-5 x V3 NaOH

No. of moles of HCl reacted with excess moles of NaOH in the reaction mixture
(No. of moles of NaOH unreacted in the reaction mixture)
NA = (0.05 x V1 x 10-3 - 5 x 10-5 x V3 NaOH) g moles

Concentration of unreacted NaOH in the reaction mixture CA= NA /V2

RESULTS AND DISCUSSIONS:

Sr. No. Time (Min.) Experimental Concentration(CA)

1 15
2 30
3 45
4 60
5 75
GRAPHS:

(3) Plot experimental and theoretical conversion versus time.

14 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-5

Kinetic Studies in a Continuous Stirred Tank Reactor

OBJECTIVE:

(a) To study the performance of a CSTR.

(b) To determine the rate constant for the given reaction at ambient temperature.
.
APPARATUS:

1. CSTR with agitator and temperature batch.

2. Pipette.
3. Burette.
4. Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

1. 0.05 N Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

2. 0.05 N Sodium hydroxide solution
3. 0.05 N HCl solution
4. 0.05 N oxalic acid solution (3.15 gm per liter of solution)
5. Phenolphthalein as indicator etc.

THEORY:

Saponification of ethyl acetate proceeds as follows:

C H 3 COO C 2 H 5 + NaOH-----🡪 C H 3 COO Na + C 2 H 5 O H

(A) + (B)🡪Products
The reactants, Ethyl Acetate and NaOH are introduced at respective volumetric feed rate of

VA and VE .
Total flow rate V in = V A+VE–(1)

Volume of the liquid in the reaction vessel is constant at V,

At the beginning of the experiment, moles of Ester and alkali changes with respect to time, is
given by.

The reaction in the reversible direction can be neglected under the specific conditions i.e. the
excess of NaOH.

15 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Working Rate Equation:

− rA=− dCA= k2 CA CB = k2 CA0 2 (1 − XA) (M − XA), where M = CB0/CA0

PROCEDURE:
● Prepare 7 litres of 0.1N NaOH solution.
● Prepare 6 litres of 0.1N Ethyl Acetate solution
● Standardize HCl and NaOH solutions (use standard Oxalic Acid of strength 0.1N)
● Transfer NaOH and Ethyl Acetate solution into two overhead tanks provided in the
experimental set up.
● Adjust the flow rates of NaOH and Ethyl Acetate to 2.5, 5, 7.5 LPH of each stream .
● Collect 10 ml sample at steady state and arrest with HCl
● The reaction mixture is titrated against NaOH.
OBSERVATION TABLE:

Sr. No. Time (min.) Volume of NaOH for back CA

titration, V3 ml
1 2
2 4
3 6
4 8
5 10
6 12
7 14
8 16
9 18
10 20
11 22

CALCULATION:

(1) Sample taken from the reactor for titration = --------- (V1 ml)
(2) Volume of HCL used to arrest the further reaction = -------- (V 2 ml) and strength (S2 N).
(3) Volume of NaOH required to titrate the excess HCl = -------- (V3 ml) and strength (S3 N).

Initial acid strength = y2 = gm equivalent /1000

Conversion XA = 1 – 1/ CA0

16 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

RESULTS AND DISCUSSIONS:

INTIGRAL METHOD OF ANALYSIS **

Plot Inverse conversus time t, yield straight line confirm second order kinetics and slope will

Gives rate constant k2 = -------- lit. / Mol min at room temperature _______0C.

17 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-6

PSEUDO–ORDER REACTIONS

OBJECTIVE:

To study pseudo first order reaction for hydrolysis of ethyl acetate.

APPARATUS:

● Batch reactor with agitator and temperature batch.

● Pipette.
● Burette.
● Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

● 0.05 M Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

● 50 mol Water
● 0.05 M Sodium hydroxide solution
● 0.05 M HCl solution
● Phenolphthalein as indicator etc.

THEORY:

A reaction in which one of the reactants is present in a large excess shows an order
different from the actual order. The experimental order which is not the actual one is
referred to as the pseudo order. Since for elementary reactions molecularity and order
are identical, pseudo-order reactions may also be called pseudo molecular reactions.

Let us consider a reaction

A + B ⎯⎯→ products

in which the reactant B is present in a large excess. Since it is an elementary reaction,

its rate law can be written as

rate = k [A] [B]

As B is present in large excess, its concentration remains practically constant in the

course of reaction. Thus the rate law can be written as

rate = k′ [A]

where the new rate constant k′ = k [B].

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 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Thus the actual order of the reaction is second-order but in practice it will be
first-order. Therefore, the reaction is said to have a pseudo-first order. Examples of
Pseudo-order Reactions

(1) Hydrolysis of an ester. For example, ethyl acetate upon hydrolysis in aqueous
solution using a mineral acid as catalyst forms acetic acid and ethyl alcohol.

CH3COOC2H5 + H2O ⎯⎯→ CH3COOH + C2H5OH

ethyl acetate (excess) acetic acid ethyl alcohol Here a large excess of water is used
and the rate law can be written as

rate = k [CH3COOH] [H2O]

= k′ [CH3COOH]

The reaction is actually second-order but in practice it is found to be first-order. Thus

it is a pseudo-first order reaction.

For Example:

Time CH3COOC2H5 H2O CH3COOH C2H5OH

(mol) (mol) (mol) (mol)

t=0 0.05 50 0 0

t 0 49.95 0.05 0.05

PROCEDURE:

● Prepare 0.05 M 300 ml ethyl acetate and 50 M 300 ml H2O

● Prepare a solution of 0.05 N 100 ml HCl and 0.05 N 100 ml NaOH solutions for the
titration.

● Use phenolphthalein as an indicator.

● Take 6 Nos. of 250 ml conical flasks and put 10 ml of 0.05 M NaOH in each flask.

● Take 0.05 M HCl solution in the burette.

● Adjust the temperature of the water bath at 40 oC.

● Take 300 ml each of 0.05 M CH3COOC2H5 and 50 M 300 ml H2O in two separate
flasks and keep these in the water bath for about 15 min to preheat the solutions.

19 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

● Transfer these solutions quickly in the batch reactor. Start immediately the mixer and
the stopwatch.

● At regular intervals of 15 min., withdraw 10 ml of reaction mixture and put it in the

conical flask containing 0.05 M NaOH. Take at least 6 samples at regular intervals of
time.

● Titrate the excess 0.05 M NaOH in each flask using 0.05 M HCl from burette and
phenolphthalein as indicator.

OBSERVATION & OBSERVATION TABLE:

● Reaction temp = oC = K
● Conc. of HCl = N3 = 0.05 M
● Conc. of NaOH (A)= N1 = 0.05 M
● Conc. of Ethyl acetate (B) = 0.05 M
● Vol. of Ethyl acetate taken = 300 ml
● Vol. of Water = 300 ml
● Initial Conc. of Ethyl acetate (A) in the mixture, CAO = 0.05 N (g mole/L)

Sr. Time Volume of Volume of sample Volume of HCL

No. (min.) NaOH taken, V1 taken for used for Titration,
ml titration, V2 ml V3 ml
1 15
2 30
3 45
4 60
5 75

CALCULATIONS:.

Estimation of un-reached Ethyl Acetate in the reaction mixture (C A)

Volume of 0.05 M NaoH taken in conical flask V1= 10 ml

Volume of reaction mixture sample added V2 = 10 ml
Volume of 0.05 M HCl used in titration for neutralization of excess 0.05 M NaoH,
V1 NaOH = ml

Reaction between NaOH and HCl is:

20 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

NaOH + CH3COOC2H5 —> CH3COONa + C2H5OH

i.e., 1 mole of NaOH reacts with 1 mole of CH3COOC2H5

RESULTS AND DISCUSSIONS:

Sr. No. Time (Min.) Experimental Concentration(CA)

1 15
2 30
3 45
4 60
5 75
GRAPHS:

(4) Plot experimental and theoretical conversion versus time.

21 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-7

Differential Method of Analysis

OBJECTIVE:

To determine the order of reaction (n) and the reaction rate constant (k) for the given
saponification reaction of ethyl acetate in aqueous sodium hydroxide solution by Differential
method of analysis
APPARATUS:

● Batch reactor with agitator and temperature batch.

● Pipette.
● Burette.
● Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

● 0.05 N Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

● 0.05 N Sodium hydroxide solution
● 0.05 N HCl solution
● Phenolphthalein as indicator etc.

THEORY:

Saponification of ethyl acetate proceeds as follows:

C H 3 COO C 2 H 5 + NaOH → C H 3 COO Na + C 2 H 5 O H

(A) + (B) → Products

The reaction in the reversible direction can be neglected under the specific conditions i.e. the
excess of NaOH.

Differential method of analyses of data

The differential method of analysis deals directly with the differential rate equation to be
tested.. The procedure is:

1. Plot the CA vs. t data, and then by eye carefully draw a smooth curve to represent the data.

2. Determine the slope of this curve (dCA /dt = rA ) at suitably selected concentration value.

22 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

3. Search for a rate expression to represent this rA vs. CA data,

● The differential method is useful in more complicated situations but requires more
accurate or larger amounts of data. The integral method can only test this or that
particular mechanism or rate form; the differential method can be used to develop or
build up a rate equation to fit the data.

PROCEDURE:

● Prepare 0.05 N 300 ml ethyl acetate and 0.05 N 300 ml NaOH.

● Prepare a solution of 0.05 N 100 ml HCl and 0.05 N 100 ml NaOH solutions for the
titration.

● Use phenolphthalein as an indicator.

● Take 6 Nos. of 250 ml conical flasks and put 10 ml of 0.05 N HCl in each flask.

● Take 0.05 N NaOH solution in the burette.

● Adjust the temperature of the water bath at 40 oC.

● Take 300 ml each of 0.05 N CH3COOC2H5 and 0.05 N NaOH in two separate flasks
and keep these in the water bath for about 15 min to preheat the solutions.

● Transfer these solutions quickly in the batch reactor. Start immediately the mixer and
the stopwatch.

● At regular intervals of 15 min., withdraw 10 ml of reaction mixture and put it in the

conical flask containing 0.05 N HCl. Take at least 6 samples at regular intervals of
time.

● Titrate the excess 0.05 N HCl in each flask using 0.05 N NaOH from burette and
phenolphthalein as indicator.

OBSERVATION & OBSERVATION TABLE:

● Reaction temp = oC = K
● Conc. of HCl = N1 = 0.05 N
● Conc. of NaOH (A)= N3 = 0.05 N

23 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

● Conc. of Ethyl acetate (B) = 0.05 N

● Vol. of Ethyl acetate taken = 300 ml
● Vol. of Sodium hydroxide = 300 ml
● Initial Conc. of NaOH (A) in the mixture, CAO = 0.05 N (g mole/L)
● Initial Conc. of Ethyl acetate (B) in the mixture, CBO = 0.05 N (g mole/L)

Consider data for 40 0C

24 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

Experiment No.-8

Integral Method of Analysis

OBJECTIVE:

To determine the order of reaction (n) and the reaction rate constant (k) for the given
saponification reaction of ethyl acetate in aqueous sodium hydroxide solution by Integral
method of analysis
APPARATUS:

● Batch reactor with agitator and temperature batch.

● Pipette.
● Burette.
● Conical flasks, thermometer, measuring cylinder etc.

CHEMICALS:

● 0.05 N Ethyl acetate solution (5 ml Ethyl acetate per liter of solution)

● 0.05 N Sodium hydroxide solution
● 0.05 N HCl solution
● Phenolphthalein as indicator etc.

THEORY:

Saponification of ethyl acetate proceeds as follows:

C H 3 COO C 2 H 5 + NaOH → C H 3 COO Na + C 2 H 5 O H

(A) + (B) → Products

The reaction in the reversible direction can be neglected under the specific conditions i.e. the
excess of NaOH.

Integral method of analyses of data

The Integral method of analysis deals directly with the Integrated rate equation to be tested..
The procedure is:

● In the integral method of analysis we guess a particular form of rate equation

and, after appropriate integration and mathematical manipulation, predict that
the plot of a certain concentration function versus time should yield a straight
line.

25 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

● The data are plotted, and if a reasonably good straight line is obtained, then the
rate equation is said to satisfactorily fit the data.
● The integral method is easy to use and is recommended when testing specific
mechanisms, or relatively simple rate expressions, or when the data are so
scattered that we cannot reliably find the derivatives needed in the differential
method.

PROCEDURE:

● Prepare 0.05 N 300 ml ethyl acetate and 0.05 N 300 ml NaOH.

● Prepare a solution of 0.05 N 100 ml HCl and 0.05 N 100 ml NaOH solutions for the
titration.

● Use phenolphthalein as an indicator.

● Take 6 Nos. of 250 ml conical flasks and put 10 ml of 0.05 N HCl in each flask.

● Take 0.05 N NaOH solution in the burette.

● Adjust the temperature of the water bath at 40 oC.

● Take 300 ml each of 0.05 N CH3COOC2H5 and 0.05 N NaOH in two separate flasks
and keep these in the water bath for about 15 min to preheat the solutions.

● Transfer these solutions quickly in the batch reactor. Start immediately the mixer and
the stopwatch.

● At regular intervals of 15 min., withdraw 10 ml of reaction mixture and put it in the

conical flask containing 0.05 N HCl. Take at least 6 samples at regular intervals of
time.

● Titrate the excess 0.05 N HCl in each flask using 0.05 N NaOH from burette and
phenolphthalein as indicator.

OBSERVATION & OBSERVATION TABLE:

● Reaction temp = oC = K
● Conc. of HCl = N1 = 0.05 N
● Conc. of NaOH (A)= N3 = 0.05 N
● Conc. of Ethyl acetate (B) = 0.05 N
● Vol. of Ethyl acetate taken = 300 ml
● Vol. of Sodium hydroxide = 300 ml

26 Prepared by : Dvarkesh Mahera

 PARUL UNIVERSITY
FACULTY OF ENGINEERING AND TECHNOLOGY
Chemical Reaction Engineering (03602360) Diploma 3rd Year

● Initial Conc. of NaOH (A) in the mixture, CAO = 0.05 N (g mole/L)

● Initial Conc. of Ethyl acetate (B) in the mixture, CBO = 0.05 N (g mole/L)

Consider data for 40 0C

27 Prepared by : Dvarkesh Mahera