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Cre Experiment. 1 To 6

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0% found this document useful (0 votes)
20 views21 pages

Cre Experiment. 1 To 6

Uploaded by

Ritesh Rai
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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Madan Mohan Malaviya University of technology

Vision

To facilitate and promote studies. research. technology incubation. product innovation and
extensionwork in Sciencc. lechnology and Management Education. and to achieve excellence in
higher technical education.

Mission

The distinctive mission of the University is:


To serve society as a centre of higher learning. providing long-term societal benefits through
transmiting advanced knowledge. discovering new knowledge. and functioning as an active
working repository of organized knowledge.
To take leadership role by providing need-based programs in engineering and technology.
applied sciences. management, hunmanities, architecture, pharmacy, retail and fashion
design. mass-communication, agriculture, and other employable courses in emerging areas.
To promote compassionate care of the highest quality that translates new knowledge into
meaningful improvements in technological outcomes through interdisciplinary
collaboration. fiscal responsibility, support of diversity, a focus on quality and a culture of
professionalism.
To establish value creating networks and foster relationship with other leading institutes of
higher learning and rescarch. alumni. and industries in order to provide significant
contribution to national and international development.
To create an intellectually stimulating Infrastructure and conducive environment for
technology research. scholarship. creativity, innovation, entrepreneurship. and profesional
activity for service to community and economy.

2
Department Vision
To become a globally leading Chemical Engineering Department by imparting quality cducation
through excellence in teaching. research, and innovation.
Mission

To provide high-quality education that will prepare the students for leading roles in their
professional jouney.
To contribute in the sustainable development of the nation and to improve the quality of life
through education. research. professionalism and leadership.
To work in collaboration with alumni and other technical institutes/universities/
industries/research organizations of national and international stature to address global
challenges in the domain of Chemical Engineering.
PROGRAM EDUCATION OBJECTIVES (PEO)
3 To inculcate with knowledge of the fundamentals of Science and Engineering disciplines for
developing the ability of students to formulate. solve and analyse the problems of Chemical
Engineering.
To assist the students in pursuit of their successful career by imparting them the lifelong
skills of creative thinking and the ability to handle problems of practical relevance to society
while complying with economic. environmental. ethical and safety factors.
To impart the knowledge about contemporary technologies. practical experiences, and soft
skills in multidisciplinary field for building up team spirit and leadership qualities by
working on multidisciplinary projects.

PROGRAM SPECIFIC OUTCOMES(PSO)


Graduate of Chemical Fngincering of Department will be able to
Demonstrate the Chemical Engineering fundamentals learnt through lectures, practical's,
and computer aided designs, projects, and field-based training.
3 Apply the knowledge of Chemical Engineering in addressing the needs of society including
environmental stewardship and to identify, analy se, design and develop solution for complex
engineering problems of practical relevance tochemical and allied industries.

3
independentPO12. engineering
in ininstructions.
PO11. effective
engineeringPO10. in norms
PO9.development.
PO8. solutions
sustainable engineering
professional
practice.
PO7. societal, engineering
PO6. an information
POS. methods PO4. design for engineering
a diverse understanding PO3.natural
fundamentals,PO2.Engineering
POT:PROGRAM
team. the
Life-long Individual Ethics: ofEnvironment The Modern Design/development
Conductpublicsystem of Problem
Communication:
Project reports the sciences, Engineering
to teams, in health,
engineer including
manage and community engineering societal and to problems
andmanagement Apply provide
tool health
components Graduates
and OUTCOME (PO)
learning: management and and and safety, of ITinvestigations andanalysis:
life-long projects design and and and the toolsusage: design and engincering knowledge: an
teamwork: in ethical engineering
multidisciplinary legal
limitations. valid reaching
and environmental
Recognize and documentation, Communicate practice. sustainability: society:includingCreate, of
safety.
or Identify. wil
learning principles with principles and conclusions.
experiments, processes
and ofsolutions:
and substantiated
be
in society Function cultural Apply predictionselect, complex the sciences. specializationApply able
multidisciplinary
inthe finance: formulate.
the and and contexts, cultural. that
to:
effectively settings. reasoning
issues, and
broadest
need apply make ateffectively commit Understand problems: meetDesign
analysis the
Demonstrate large., and apply
4
for conclusions knowledge
these effective and and modelling societal.solutions
the review to
and such to informed appropriate and the
context
environments. on as demonstrate the the specified
have to professional interpretation Use solution
complexas. an consequent and research
one'presentations,
s impact research-based
change. ofthe knowledge
technological being individual, by to environmental for using of
needs
preparation own the complex
techniques, complex mathematics, of
engineering the ofcontextual literature.
firstcomplex
work, able ethics responsibilities with
knowledge the of
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understanding
and give as resources, considerations. and science,
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and relevant activities synthesisconsiderationmathematics,
engineering and and engincering
to and writeand with or
problems.
engage leader of need to modern research complex
leader assess
to of
the the and for the with the
Contents
8 4 3 2
ContentsNo. S.

Continuous tank Law Study Batch BatchPseudoreaction


Arrhenius
Plug stirred
reactor
flow Second
order

reactor:
of reactor:
second First
order Chemical
PseudoSecond
order
reaction
reaction first order Reaction
reactor
order
reaction
for
reaction
unequal Engineering-I

concentration

Lab
(BCT
of
reactants 28A)

PageNo
26 23 21 19 16 13 10 7
reaction
vessels, notspecifically
A Chemical
relates in
homogeneous
present chemical
kineticsretorts,
industrialreaction
by engineering or
is
certain itself.
or
also
heterogeneous engineering
considered fuel but
rather
cells, catalytic to About
is
asintegrated
and catalyst (reaction
an chemistry Chemical
integral
photocatalytic
is
intopresent
engineering
part. dealing Reaction
a
process, reaction in
surfaces. the with
Engineering
or
reactor. chemicalreactor
for
The
example systems
Sometimes
issue engineering)
reactors.
of in
reactive
solvent Frequently
either.
awhere
reactor
is
separations
effectson a
per specialty
the
se term
is
Experiment No: 1

Title: Second Order Reaction


Aim: To findorder of reaction by integral method of analysis
Chemicals: Ethyl Acetate. NaOH. HC. Phenolphthalein.

Theory:
Integral Method of Analysis of Data
General Procedure: The integral method of analysis always puts a particular rate equation to the
test by integrating and comparing the predicted C versus t curve with the experimental C versus t
data. If the fit is unsatisfactory, another rate equation is guessed and tested.
Ii should be noted that the integral method is especially useful for fitting simple reaction types
corresponding to elementary reactions. Let us take up these kinetic forms. Irreversible Unimolecular
Type First-Order Reactions. Consider the reaction
A ’ Products

Suppose we wish to test the first-order rate equation of the following type.
dCA
-rA= dt
= kCA

for this reaction. Separating and integrating we obtain


Ca dCA
= k| dt
JCA0 CA
Or.

- In
CA = kt
CA0
If A plot of -In (C/CAo) vs. tgives a straight line through the origin, the reaction is first order. If
the experimental data seems to be better fitted by a curve than by a straight line, try for second order
rate form because the first-order reaction does not satistactorily fit the data. Thus, for the second
order reaction with equal initial concentrations of A and B, or for the reaction
2A ’ Products
Thedefining second-order differential equation becomes
-rA= dCa = kC' kCao(1-X)²
dt

Which on integration yields


1 1 1 X¡
= kt
Ca CA0 CA01 - XA
Plotting the graphwith
CA
time as shown in ig. provides atest for this rate expression.

1/CA

booo Slope = k
1
CAO

Procedure:
PART A: (Standardisation)
1. Titrate 10ml 0.1N Oxalic Acid with reactant NaOH solution.
2. Calculate normality of reactant NaOH solution. N2
3. Titrate 10ml Oxalic Acid with burette NaOH solution.
4. Calculate normalityof burette NaOH solution i.e. Ni
PART B: (Kinetics)
1. Take five conical flasks A. B. C. D and E. (clean it)
2. In each conical flask add 1Oml of given 0.IN HCI solution and indicator.
3. In a beaker take 100ml 0.IN Ethyl acetate.
4. In that beaker add 100m/reactantNaOH and start stopwatch.
5. After 2min from start of reaction take 20m/ of reaction mixture by pipette and
add it in
conical flask A'.
6. After 5min from start of reaction take 20ml of reaction mixture by pipette and add
it in
conical flask B.
7. After 10min from start of reaction take 20ml of reaction mixture by pipette and add
it in
conical flask C"
8. After 15min from start of reaction take 20ml of reaction mixture by
pipette and add it in
conical flask D'.

8
add it in
from start of reaction take 20m/ of reaction mixture by pipette and
9. After 20min
conical flask E',
mixture with given 0.01N NaOH.
10. Titrate conical flasks A. B. C, D and E

Observation Table:
1
CA
CA
Time (min) Burette Reading (ml) CA

10

15

20

Formula:
CA=(HCVHCI-(BR)XNBRY
VR

Where.
NHCI =the normality of HCI solution
VHI= the volumeofHClsolution (m/)
VR= Volume of sample of reaction mixture taken for titration (l)
BR = Volume of NaOH required for titration of reaction mixture sample (ml)
NBR = Normality of NaOH (in burette) used for titration of reaction sample

Conclusions:

1. As a plot of -In()
CA0
vs. time I, is not a straight line, the reaction not first order.
1
2. As aplot of graph CA with time tgives straight line, the reaction is second order.

Results:

1. CAU N/2 ---(by titration)


2. CA ---(from the intercept inthe graph)
3. Rate constant k
(Slope from the graph)

9
Experiment No: 2
Title: Pseudo First Order Reaction
Aim: Tostudy pseudo first order reaction
Chemicals: Ethyl Acetate. NaOH, HCI. Phenolphthalein.

Theory:
Pseudo First Order Reaction
A+ B’C+D
When reaction is bimolecular and one of the reactants
(volume) is in excess with respect to other
reactant, the change in concentration of that excess reactant is
negligible with time and reaction rate
is dependent upon only limiting reactant. This is called
Pseudo First Order Reaction.
-Ta = kCA Cg
As Cg > C¡
Thechange in CB is negligible with reaction time
Therefore

-T = k,CA
Where. k, = kCg
And reaction becomes Pseudo First
Order Reaction which can be represented as
A ’ Products
Suppose we wish to test the first-order rate
equationof the following type,
dCA
-rA=
dt
= kCA
for this reaction.
Separating and integrating we obtain
CA dCA
Or JCAO CA

-In CA0CA kt
IfAplot of -In (C/CAo) Vs. t gives a
straight line through the origin, the
reaction is first order.
Procedure:
PART A: (Standardisation)
1. Titrate 1Om/0.IN Oxalic Acid
with reactant NaOllsolution.
10
2. Calculate normality of reactant NaOH solution, N,
3. Titrate 1Om/ Oxalic Acid with burette NaOH solution.
4. Calculate normality of burette NaOH solution i.e. Ni

PART B: (Kinetics)
1. Take five conical flasks A, B. C, D and E.(clean it)
2. Incach conical flasks add 10m/ of given 0.I N HCIsolution and indicator.
3. In abeaker take 25 ml 0.IN Ethyl acetate.
4. In that beaker add 250 ml reactant NaOH and start stopwatch.
5. After 2min from start of reaction take 20ml of reaction mixture by pipette and add it in
conical flask A'.
6. After Smin from start of reaction take 20ml of reaction
mixture by pipette and add it in
conical flask B,
7. After 10min from start of reaction take 20ml of
reaction mixture by pipette and add it in
conical flask C'.
8. After 15min from start of
reaction take 20ml of reaction mixture by pipette and add it in
conical flask D'.
9. After 20min from start of
reaction take 20ml of reaction mixture by pipette and
add it in
conical flask 'E'.
10. Titrate conical flasks A,B.C, Dand E
mixture with given 0.01N NaOH.
Observation Table:
Time (min) Burette Reading (ml) CA
CA 1

2
-ln CAO

15

20

Formula:

C= (NucoxVnc-(BR) XNBR}
VR
11
Where.
NHCI= the normality of HCl solution
VHCI =the volume of HClsolution (m)
VR = Volume of sample of reaction mixture taken for titration (ml)
BR=Volume of NaOH required for titration of reaction mixture
sample (ml)
NBR= Normality of NaOH (in burette) used for titration of reaction
sample.
Results:
1. CA0 =N2/2 ---(by titration)
2. Rate constant k=
(Slope from the graph)
Conclusions:
1. As a plot of -In (C/CAo) vs.
time is a straight line, the reaction is
2. As a plot of graph with
1
first order.
time is not a straight line, the
CA
reaction is not second order.
Experiment No: 3
Title: Bateh reactor: Second order reaction
Aim: To calculate theoretical time of reaction by design equation for batch reactor
Chemicals: Ethvl Acetate. NaOH.

Theory:
Derivation of design cquation of Batch reactor
Material Balance equation for batch reactor is as follows:
=0

Aput= 9átput + Disappearance + Accumulation

Rate of loss of reactant A within Rate of accumulation of


reactor due to chenmical reaction reactant A within the reactor

Evaluating the terms of Eq. 1, we find


Disappearance of A moles Areacting
by
reaction, (moles/
a time)(volume of fhuid (volume of fluid)

Accumulation of dNA d[NA0(1 - X¡)] dXA


A, (moles/time) dt dt -NA0 dt
By replacing these two terms in Eq.1, we obtain

-(r)V= NAo dXdt


Rearranging and integrating then gives
XA dXA
t=
-(r)V
This equation may be simplified for a number of
situations. If the density of the fluid remains
constant, we obtain

dXA CA dCA
t= Cao -(r) -(r) fore, = 0

13
Graphical method of finding theoretical time:

1
Area =!

CA CAO
For the second-order reaction with equal initial concentrations of Aand B, or for the
reaction
2A ’ Products

1 1 1 XA
= kt
CA CAO CAO 1 - XA

Procedure:
PART A: (Standardisation)
1. Titrate 10ml 0.IN Oxalic Acid with
reactant NaOH solution.
2. Calculate normality of reactant NaOH solution. N2
3. Titrate 10ml Oxalic Acid with burette NaOH
solution.
4. Calculate normalityof burette NaOH
solution i.e. N,
PART B: (Kinetics)
1. Take five conical flasks A, B, C, D
and E. (clean it)
2. In cach conical flask add 10ml of given
0.IN HCI solution and indicator.
3. In a beaker take 200m/0.1N EA.
4. In that beaker add 200 ml
reactant NaOH and start stopwateh.
5. After 2min from start of
reaction take 20ml of reaction mixture by pipette and add
conical flask 'A'. it in
6. After 5min from start of
reaction take 20m/ of reaction mixture by pipette and add it in
conical flask B'.
7. After 10min from start of
reaction take 20ml of reaction miture by
conical flask "C'. pipette and add it in

14
8. After 15nmin from start of reaction take 20m/ of reaction mixture by
pipette and add it in
conical flask D'.
9. After 20min from start of reaction take 20ml of reaction mixture by
pipette and add it in
conical flask E'.
10. Titrate conical flasks A.B.C, D and E mixture with given 0.0IN
NaOH.
1
11. Plot graph of v/st. And find value of k.
CA

PART C: (TheoreticalTime Calculation)


1. Calculate rate of reaction for different
concentrations by using 'k' calculated from above
graph.
2. Calculate 1/(-rA) for different CA
3. Plot graph of 1/(-rA) Vs CA
4. Calculate the area under the curve between
boundaries CAo to Ca, which is the theoretical
time
Observation Table:
PART AJ (Standardisation)
Volume (in flask ml) Burette Reading (m) Normality (N)
N=

PART B] (Kinetics)
Time (min) Conductivity CA

CA

PART C]: (Theoretical time calculation)


CA
Rate (-rA) 1
-rA

Results:
1. Theoretical time = min
(area under the curve)
2. Actual time min

15
EXPERIMENT No: 4
Title: Batch reactor: Pseudo First Order Reaction
Aim: To calculate theoretical time of reaction by design equation for batch reactor
Chemicals: Ethyl Acetate, NaOH.

Theory:
Derivation of design equation of Batch reactor
Material Balance equation for batch reactor is as follows:
=0

iput= Oátput + Disappearance + Accumulation


Or

)
Rate of loss of reactant A Rate of accumulation of
within reactor due to reactant A within the reactor (1)

Evaluating the terms of Eq. 1, we find


Disappearance of A moles Areacting
by :-(ra)V= (
reaction,(moles/ (time) (volume of fluid)')(volume of fluid)

Accumulation of dNA d[N o(1 X)]


A, (moles/time) dt dt -N 0 dXA
dt
By replacing these two terms in Eq.1, we obtain

-(r)V= NA0 dx4


dt
Rearranging and integrating then gives
t= Na0 dXA
Jo -(ra)V
This equation may be simplified for a number of
constant, we obtain
situations. If the density ofthe fluid remains
Xa dXA Ca dCA
-(r) forea = 0

16
Graphical method of finding theoretical time:

Area = 1

CA
For Pseudo First Order Reaction.

CA =kt
-In
CA0
Procedure:
PART A: (Standardisation)
1. Titrate 10ml 0.IN Oxalic Acid
with reactant NaOH solution.
2. Calculate nornmality of reactant NaOH
solution. N2
3. Titrate 10ml Oxalic Acid with burette
NaOH solution.
4. Calculate normality of burette NaOH
solution i.e. NI

PART B: (Kinetics)
1. Take five conical flasks A, B. C.
D and E. (clean it)
2. In each conical flask add 10 m/ of
given 0.IN HCI solution and indicator.
3. In abeaker take 200 ml 0.IN
ethyl acetate.
4. In that beaker add 200 ml
reactant NaOH and start slopwatch.
5. Afler 2 min from start of
reaction take 20ml of reaction nmixture by
conical flask 'A'. pipelte and add it in
6. After 5 min from start of
reaction take 20ml of reaction mixture by
conical flask B'. pipete and add it in
7. After 10min from start
of reaction take 20ml of
conical lask " reaction mixture by pipette and add it in
8. After 15 min from start of
reaction take 20ml of reaction mixture by
conical flask D'. pipette and add it in

17
9. After 20 min from start of reaction take 20m/ of reaction mixture by pipette and add it in
conical flask E'.
10. Titrate conical flasks A, B. C. D and E mixture with given 0,0|N NaOH.
l1. Plot graph of -In (Ca/CAo) v/s t.and find value of k.

PART C: (TheoreticalTime Calculation)


1. Calculate rate of reaction for different concentrations by
using 'k calculated from above
graph.
2. Calculate 1/(-rA )for diferent C
3. Plot graph of 1/(-rA) Vs Ca.
4. Calculate the area under the curve between
boundaries CAo to CA. which is the theoretical
time.

Observation Table:
PART A] (Standardisation)
Volume (in flask ml) Burette Reading (m) Normality (N)
N=

PART B] (Kinetics)
Time (min)
Conductivity CA
-ln CA
CA0

PART C: (Theoretical time ealeulation)


CA
Rate (-rA) 1

Results:
1. Theoretical time Mn
(area under the curve)
2. Actual time min

18
Experiment No. 5
Title: Study of Second Order Reaction for UnequalConcentration of Reactants
Aim: To findorder of reaction by integral method of analysis
Chemicals: Ethyl Acetate. NaOH.

Theory:
Consider the reaction
A+ B ’ Products
With corresponding rate equation

-rA =
dCA dCB = kCaCB
dt dt
Noting that the amounts of A and B that have reacted at any
time t are equal and given by CAoX
.we may write equation as in terms of X as

-TA = C 0 dXA
dt = k(C 0 - CA0XA)(Cgo - CA0Xa)
Let M = CB/CAO be the initial molar
ratio of reactants, we obtain
-rA = CA0 dX = kCAo (1- X)(M -X¡)
dt
Which gives,
rA
dXA
(1- X) (M - X) =CAok dt
After breakdown into partial
fractions, integration, and rearrangenment, the final result in a number
of different forms is

1- X = In M XA
In
1- XA M(1 - X) = In CpCAo = In =
M#1
ChaCa MCA CAo(M - 1)kt = (CB0 - CAo) kt,
Figure shows two equivalent ways of
obtaining a linear plot between
time for this
second-order rate law. theconcentration function and

lotercept In

19
Procedure:
PART A: (Standardisation)
Titrate 10ml 0, IN Oxalic Acid with reactant NaOHsolution.
2. Calculate normality of reactant NaOH solution. N:
3. Titrate lOmlOxalic Acid with burette NaOH solution.
4. Calculate normality of burette NaOH solution i.e. Ni
PART B: (Kineties)
1. Take five conical flasks A. B. C. D and E. (clean it)
2. In each conical flask add 1Oml of given 0.IN HCl solution and indicator.
3. In abeaker take 50ml 0. IN ethyl acetate.
4. In that beaker add 150ml reactant NaOHand start stopwatch.
5. After 2min from start of reaction take 20nl of reaction mixture by pipette and add it in
conical flask 'A`.
6. After Smin from start of reaction take 20ml of reaction mixture by pipette and add it in
conical flask B'.
7. After 10min from start of reaction take 20ml of reaction mixture by pipette and add it in
conical flask C'.
8. After 15min from start of reaction take 20ml of reaction mixture by pipette and add it in
conical flask D'.
9. After 20min from start of reaction take 20nl of reaction mixture by pipette and add it in
conical flask E.
10. Titrate conical flasks A, B, C, D and E mixture with given 0.01 N NaOH.
11. Plotgraph of In Ce/Ca v/s t and find value of k.

PART Aj (Standardisation)
Volume (in flaskml) Burette Reading (m/) Normality (N)
N=

PART B) (Kinetics)
Time (min) CA Ca= CRo -CAo+CA CB

Result:

1. Theoretical M=
2. Experimental M =
3. Rate constant k =

20
Experiment No. 6
Title: Arrhenius Law
Aim: To find out activation energy and frequency factor of the chemical reaction
Chemicals: Ethyl Acetate, NaOH. HCI, Phenolphthalein.

Theory:
For many reactions. and particularly elementary reactions. the rate expression can be written as a
product of a temperature-dependent term and a composition dependent term.
r;=fi(temperature). fz (composition)
For such reactions the temperature-dependent term. the reaction rate constant, has been found in
practically all cases to be well represented by Arrhenius' law:
k= ko e-E/RT
Where ko. is called the frequency or pre-exponential factor and Eis called the activation energy of
the reaction.

Sope R

Procedure:
PART A: (Standardisation)
1. Titrate 10 ml 0.1N Oxalic Acid with
reactant NaOH solution.
2. Calculate normality of reactant NaOH solution, Ni
PART B: (Kinetics)
1. Take 3 beakers and 3 conical flasks A, B
and C.
2. In each beaker add 50ml of 0.IN EA
solution.
3. In each conical flask add 50ml of
reactant NaOH solution.
4. Keep 'A' beaker and A' conical flask in hot
water bath at 40'C for ISmins at constant
temperature.

21
5. Keep B beaker and B' conical flask in hot water bath at 50'C for 15mins at constant
temperature.
6. Keep c beaker and C' conical flask in hot water bath at 60°C for 15mins at constant
temperature.
7. Mixthe respective reactants and keep it in water bath for Smins. (dt)
8. Take 20ml of reaction mixture and add 10m/ 0.IN HCIto it.
9. Titrate the mixture A, B, C with 0.0IN NaOH
Observation Table:
Temperature (°C) Burette Reading (ml) CA
k=
dCa 1
dt CA2
40
50
60

Temperature (K) 1 In k
T

Formula:

Ca= (NH|x VHCI-(BR) XNBR


VR

Where.
NHCI=the normality of HCI solution
VHCI =the volume of HCI solution (m)
VR= Volume of sampleof reaction mixture taken for titration (n)
BR=Volume of NaOH required for titration of reaction mixture sample (nn)
NuR = Normality of NaOH(in burette) used for titration of reaction sample

Graph:
Plot a graph of In k v/s I/T
Result:

1. Activation Energy E
(rom graph)
2. Frequency Factor ko =
(lrom graph)
22

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