Department of Chemical

Engineering university of
Engineering and Technology
Peshawar.

Lab
Report
Chemical
Reaction
Engineering

By: UBAID ULLAH JAN

Reg No: 19PWCHE1455
Section: C
Semester: 6 th

To: Sir, Engr Murtaza Khan

 TABLE OF CONTENTS
S.No TOPICS PAGE
01 Demonstration of Chemical Reactor Service Unit

CALIBRATION OF FEED PUMPS, TEMPERATURE AND

CONDUCTIVITY SENSORS PROVIDED WITH CHEMICAL
02 REACTOR SERVICE UNIT AND TO FIND OUT FLOW RATE AT
VARIOUS POTENTIOMETER SPEED.
03 Demonstration of Batch reactor

To derive a relationship between conductivity and concentration

04 for batch sponification of ethyl acetate
To determine the order and rate constant for batch
sponification of ethyl acetate

TO DETERMINE THE ORDER AND RATE CONSTANT FOR

05 BATCH SPONIFICATION OF ETHYL ACETATE

06 Demonstration of Continuous stirred tank reactor

07 To determine the order and rate constant for sponification of

ethyl acetate using continuous stirred tank reactor

08 To determine the effect of inadequate mixing on reaction rate in

continuous stirrer tank reactor unstirred reactor with baffle
and unstirred reactor without baffle.
09 To find the effect of flow rate on reaction rate using
continuous stirred tank reactor

10 Demonstration of tubular (plug flow reactor) reactor

11 To determine the rate constant and order of reaction for saponification

of ethyl acetate using half-life method using PFR

1
 Experiment No 01:
Demonstration of Chemical Reactor Service Unit

This unit is designed by internationally modified UK Company, ARMFIELD. Its basic material
of construction is ABS (Acronytrile-Butadiene-Styrene).

SPECIFICATIONS

It is basically a self contained bench top service unit designed in such a manner that three
types of reactors can be mounted on it:
 Batch reactor
 Tubular reactor
 Stirred tank reactor

REAGENT TANK

There are two reagent tanks on the unit having a capacity of 5 liters each. They are used to
store the reactants. There are rigid pipes inside the tanks that are used to suck the reactants
from the tanks.

PUMPS

There are two peristaltic pumps, one for each reagent tank. They work as feed pumps for the
reactor and transfer reactants from the tank to reactor. The speed of these pumps can be
changed using controllers beside them. The flow rate from the pump ranges from 0-95 ml/min.

AGITATOR SPEED CONTROLLER

Agitator is driven by electric motor and is used for homogenization of heat in the reactor. The
speed of agittor can be controlled using control system, at the right side of the pumps.

HOT/COLD WATER CIRCULATOR FOR REACTORS

It usually provides hot or cold water for the reactor. Water is heated in the circulator by electrical
heating.

AUTOMATIC TEMPERATURE CONTROL

Temperature is sensed and controlled using automatic temperature control. Temperature

control is achieved by heated/cooled water in the coil inside the reactor.

CONDUCTIVITY MEASUREMENT

There is a conductivity probe which can be used with any of the reactors. During the chemical
reaction, it senses the conductivity of the solution and conductivity values are displayed on the
screen.a

2
 EXPERIMENT # 2
CALIBRATION OF FEED PUMPS, TEMPERATURE AND CONDUCTIVITY SENSORS
PROVIDED WITH CHEMICAL REACTOR SERVICE UNIT AND TO FIND OUT FLOW RATE
AT VARIOUS POTENTIOMETER SPEED.

EQUIPMENTS USED:
 Chemical reactor service unit equipped with;
 Reagent tanks
 Temperature and conductivity sensors

DEMONSTRATIONS

TEMPERATURE CALIBRATION
Took the temperature sensor, plugged it in chemical reactor service unit and switched on
the temperature reading meter. Kept the sensor in air for few minutes to measure the
room temperature. Then put the sensor in water for a minute to measure the water
temperature. Temperature was shown on the temperature meter on the service unit.

CONDUCTIVITY CALIBRATION
Plugged the conductivity sensor into the service unit and switched on. Took a beaker and
filled with water. Put the sensor in plain water and measured the conductivity displayed on
the conductivity meter on the service unit.
Then made a salt solution in water in the beaker. Put the conductivity sensor in the salt
solution and then measured the conductivity. Noted the difference between the
conductivity of plain water and that of salt solution.

FLOW RATE AT VARIOUS POTENTIOMETER SPEEDS

First checked that all measuring probes and reagent tanks were connected to chemical
reactor service unit. Filled the reagent tanks with water fitted on the service unit. Switched
on the service unit and checked that all the components were working properly. Sat the
potentiometer speed by variable speed controller fitted on the service unit. Took a beaker;
put the silicon tube pipe in it which is connected to peristaltic pump. Switched on the pump.
Noted the flow of water with respect to time. Then calculated the flow rate by the formula,
Q= Volume in ml
Time (min)
Similarly calculated different flow rate at different potentiometer speed.
Finally plotted a graph between flow rate and potentiometer speed by taking flow rate on Y-
axis and potentiometer speed on X-axis.

3
 OBSERVATION AND CALCULATIONS
TEMPERATURE CALIBRATION

1. Room temperature = 300C

2. Water temperature = 28.90C
3. Air temperature = 26.50C

CONDUCTIVITY CALIBRATION

1. In simple water = 0.58 mS

2. On salt solution = 6.72 mS

FLOW RATE AT VARIOUS POTENTIOMETER SPEED

S.NO Potentiometer Speed Volume (ml) Time (sec) Flow rate

V t Q=V/t
1 3 50 178 16.85
2 4 50 106.87 28.10
3 5 50 77.44 37.74
4 6 75 94.45 47.64
5 7 75 76.48 58.84
6 8 75 65.43 68.77
7 9 100 76.42 78.51
8 10 100 67.77 88.53

FLOW RATE vs. POTENTIOMETER SPEED

4
Experiment no 03
Demonstration of Batch Reactor
A batch reactor is a simple reactor that holds the components which reacts to form a
product.

BASIC CONSTRUCTION AND COMPONENTS

REACTOR VESSEL

A batch reactor usually consists of a reactor vessel which is

made of glass. The glass vessel is covered by a stainless steel
cover and there is a vacuum insulation between glass vessel
and steel cover for negligible heat loss during the process.
SPRING
There is a spring attached with the reactor and is made of
aluminum. The spring is used for holding the reactor on the
base plate which is then fitted on the chemical reactor service
unit through thumb nuts.

SPRING COIL
The reactor is equipped with stainless steel coil to which water
circulator of chemical reactor service unit is connected. This coil is
used for maintaining the temperature throughout the process.

AGITATOR
There is a propeller agitator in the reactor which is used for heat transfer and provides
good mixing of reacting components.

BASIC OPERATIONS IN THE BATCH REACTOR

1.ISOTHERMAL BATCH OPERATION
In this operation, constant operating temperature is obtained by automatically
adjusted temperature controller.

2.ADIABATIC BATCH OPERATION

This operation allows negligible heat transfer through the reactor which is done
by effective vacuum insulation surrounding the reactor wall.

DEMONSTRATION CAPABILITIES
 Batch reactor is designed to determine the reaction rate constant as well as
various changes to process conditions such as reaction temperature,
concentration, heat rate etc.
 The reactor is designed in such a way that no reagent should be used to carry
out reactions because of material of construction of reactants, temperature and
pressure.

5
EXPERIMENT NO 4
Objective:
TO DERIVE A RELATIONSHIP BETWEEN CONDUCTIVITY AND CONCENTRATION FOR
BATCH SPONIFICATION OF ETHYL ACETATE.

EQUIPMENTS USE
Batch reactor fitted on chemical reactor service unit
 Beakers,
 flasks and
 pipette for preparing the solutions

CHEMICALS USED

1. 0.1 M NaOH of 0.5 L solution

2. 0.1 M CH3COOC2H5 of 0.5 L solution

REACTION INVOLVED

The reaction involved is the batch sponification of ethyl acetate.

CH3COOC2H5 + NaOH CH3COONa + C2H5OH

PROCEDURE

Prepared 0.1 molar solution of sodium hydroxide and ethyl acetate each. After that, put 0.1M
ethyl acetate solution in the batch reactor. Noted the initial readings. Then put 0.1 M sodium
hydroxide solution in the batch reactor and started it. Started the stop watch as the NaOH
solution was poured into the reactor. Noted the conductivity readings after every two minutes
i-e regular interval of time.
Kept on taking the reading until the conductivity become constant. When the conductivity
become constant, then stopped the process. Noted all the experimental data.
Then calculated the concentration at any time’t’ is given by,

Where
CA (t) = concentration at any time t
CA (0) = initial concentration
K (t) = conductivity at any time t
K (0) = initial conductivity
K (∞) = conductivity at time t=∞

Finally plotted a graph between concentration and conductivity to relate a

relationship between them.

6
OBSERVATIONS AND CALCULATIONS
1. NaOH SOLUTION

To prepare 0.1 molar NaOH of 0.5 L solution,

No. of moles of NaOH required = molarity * volume
Thus,
nNaOH = 0.1*0.5 = 0.05 moles
Now,
1mole NaOH requires = 40 gm
0.05 mole NaOH requires = 4*0.05
= 2 grams
Thus 2 gm NaOH are required to prepare 0.1 M NaOH of 0.5 L solution.

2. ETHYL ACETATE SOLUTION

As ethyl acetate is in liquid form, so we have to determine its volume required to

prepare 0.1 Molar solution.

As, Density = mass / volume

So, volume = mass / Density
And volume = (No. of moles * Mol. wt) / Density

Now, density of ethyl acetate = 0.9 gm / ml

Thus, volume = (0.1*88) / 0.9
So, volume = 9.8 ml / L

This means that

1L solution requires = 9.8 L ethyl acetate
So 0.5 L requires = 0.5*9.8 L ethyl acetate
= 4.8 L ethyl acetate

7
 EXPERIMENTAL DATA
S.NO Time(sec) Conductivity CA XA
1 0 9.44 0.1 0
2 2 7.66 0.066914 0.330855
3 4 6.58 0.04684 0.531599
4 6 5.97 0.035502 0.644981
5 8 5.57 0.028067 0.719331
6 10 5.3 0.023048 0.769517
7 12 5.09 0.019145 0.80855
8 14 4.93 0.016171 0.83829
9 16 4.8 0.013755 0.862454
10 18 4.71 0.012082 0.879182
11 20 4.62 0.010409 0.895911
12 22 4.55 0.009108 0.908922
13 24 4.49 0.007993 0.920074
14 26 4.44 0.007063 0.929368
15 28 4.4 0.00632 0.936803
16 30 4.36 0.005576 0.944238
17 32 4.33 0.005019 0.949814
18 34 4.3 0.004461 0.95539
19 36 4.27 0.003903 0.960967
20 38 4.25 0.003532 0.964684
21 40 4.23 0.00316 0.968401
22 42 4.21 0.002788 0.972119
23 44 4.2 0.002602 0.973978
24 46 4.18 0.00223 0.977695
25 48 4.17 0.002045 0.979554
26 50 4.16 0.001859 0.981413
27 52 4.14 0.001487 0.98513
28 54 4.13 0.001301 0.986989
29 56 4.12 0.001115 0.988848
30 58 4.11 0.000929 0.990706
31 60 4.11 0.000929 0.990706
32 62 4.1 0.000743 0.992565
33 64 4.09 0.000558 0.994424
34 66 4.09 0.000558 0.994424
35 68 4.08 0.000372 0.996283
36 70 4.07 0.000186 0.998141
37 72 4.07 0.000186 0.998141
38 74 4.07 0.000186 0.998141
39 76 4.06 0 1
40 78 4.06 0 1
42 80 4.06 0 1

8
CONCENTRATION vs. CONDUCTIVITY

CONVERSION vs. CONDUCTIVITY

9
 CONCETRATION vs. TIME

RESULTS
The following relation ships have been obtained
1. The concentration decreases as the conductivity decrease so there is a direct
relation ship between concentration and conductivity.
2. The conversion increases as the conductivity decrease so there is an inverse
relation ship between conversion and conductivity.
3. The conductivity decreases with respect to time.

10
 EXPERIMENT NO 05
TO DETERMINE THE ORDER AND RATE CONSTANT FOR BATCH SPONIFICATION OF
ETHYL ACETATE

EQUIPMENTS USED
 Batch reactor fitted on chemical reactor service unit
 Beakers, flasks and pipette for preparing the solutions

CHEMICALS USED
 0.1 M NaOH of 0.5 L solution
 0.1 M CH3COOC2H5 of 0.5 L solution

REACTION INVOLVED
The reaction involved is the batch sponification of ethyl acetate.

CH3COOC2H5 + NaOH CH3COONa + C2H5OH

PROCEDURE
Prepared 0.1 molar solution of sodium hydroxide and ethyl acetate each. After that, put ethyl
acetate solution in the batch reactor. Noted the initial readings. Then put 0.1 M sodium
hydroxide solution in the batch reactor and started it. Started the stop watch as the NaOH
solution poured into the reactor. Noted the conductivity readings after every two minutes i-e
regular interval of time.
Keep on taking the reading until the conductivity become constant. When the conductivity
become constant, then stopped the process. Noted all the experimental data.
Then calculated the concentration at any time’t’ is given by,

Where
CA (t) = concentration at any time t CA (0) = initial concentration
K (t) = conductivity at any time t K (0) = initial conductivity
K (∞) = conductivity at time t=∞

DETERMINATION OF ORDER AND RATE CONSTANT

The order and rate constant can be calculated by any method including integral method of
analysis, half life, fractional life, differential method etc.

Here the method used is the differential method; According to this method;
1. Determined the concentration at each time interval and obtained a concentration
data.
2. Plotted time vs. concentration data on x and y-axis respectively.
3. Carefully drawn a smooth curve among the points obtained by the time vs.

11
 concentration data.
4. Drawn tangents at each point. That tangents represented the rate of reaction at those
points.
5. Then used the nth order rate equation;

n
-rA = kC A
Or
log (-rA) = log (k) + n.log (CA)

Which resembles to a straight line equation y = mx + c

6. Then put the data of log (-rA) and log (CA) on y and x-axis respectively.
7. Drawn a straight line among the possible data points.

OBSERVATIONS AND CALCULATIONS

EXPERIMENTAL DATA

Time Conductivity Concentration

0 9.78 0.1
2 7.2 0.054497354
4 6.28 0.038271605
6 5.74 0.028747795
8 5.38 0.022398589
10 5.14 0.018165785
12 4.96 0.014991182
14 4.82 0.012522046
16 4.71 0.010582011
18 4.62 0.008994709
20 4.55 0.007760141
22 4.49 0.00670194
24 4.44 0.005820106
26 4.4 0.005114638
28 4.36 0.004409171
30 4.33 0.003880071
32 4.3 0.00335097
34 4.28 0.002998236
36 4.26 0.002645503

12
38 4.24 0.002292769
40 4.22 0.001940035
42 4.21 0.001763668
44 4.2 0.001587302
46 4.19 0.001410935
48 4.18 0.001234568
50 4.17 0.001058201
52 4.16 0.000881834
54 4.15 0.000705467
56 4.15 0.000705467
58 4.14 0.000529101
60 4.14 0.000529101
62 4.13 0.000352734
64 4.13 0.000352734
66 4.12 0.000176367
68 4.12 0.000176367
70 4.12 0.000176367
72 4.11 0
74 4.11 0
76 4.11 0
78 4.11 0

13
Selecting the points
Time 0 2 10 20 30 40
Concentration 0.1 0.054497354 0.018165879 0.00776 0.00388 0.00194

T CA rA Log(CA) Log(-rA)
0 0.1 (0.1-0.028)/(0-2) = - 0.036 -1 -1.444
2 0.054497354 (0.076-0.012)/(0-6) = -0.0107 -1.2636 -1.97
10 0.018165879 (0.024-0.004)/(7-18) = - 0.00182 -1.741 -2.74
20 0.0076 (0.014-0.002)/(10-28) = - 0.00067 -2.11 -3.174
30 0.00388 (0.01-0)/(10-40) = - 0.00033 -2.41 -3.48
40 0.00194 (0.004-0)/(26-50) = -0.000167 -2.512 -3.78

14
The first three points seems to be in straight line so,
Slope = n = (y2 – y1)/(x2 – x1)
Here
x1 = 0 and x2 = -1.741
y1 = 0.41 and y2 = -2.74
Thus,
Slope n = (-2.74-0.41) / (-1.741 – 0)
So n = 1.81
And intercept is,
log(k) = 0.41
k = 2.57
Thus, rate constant = k = 2.57 and order = n = 1.81
So we have equation as,
1.81
-rA = 2.57 CA

15
Experiment No 06

Demonstration of Continuous Stirred Tank Reactor

It is basically a small scale reactor with an adjustable
volume of 0.4 - 1.5 liters.

BASIC CONSTRUCTION AND

COMPONENTS
VESSEL AND AGITATOR
The reactor consists of a vessel which is equipped with a
variable speed square blade turbine agitator with a speed
range 0-230 rpm.
The agitator blade usually has greater size than that of
batch reactor. This is used for efficient mixing of the
reacting components.

VESSEL CONSTRUCTION AND BAFFLE

The vessel is constructed from borosilicate glass and PVC with stainless steel heat transfer coil
and removable reactor baffle.

The main purpose of baffle is to increase the heat transfer area.

GLANDS

Glands are mounted in the lid for fitting appropriate sensors.

PILLARS

The vessel is mounted on a PVC base plate through the pillars which fits directly onto the
service unit.

16
 DEMONSTRATION CAPABILITIES:

The main aim of the continuous stirred tank reactor is the:

 Determination of reaction rate constant

 Variation of conversion with residence time
 Evaluation of empirical rate expressions from experimental data
 Effect of temperature and mixing efficiency on reaction kinetics
 Residence time distribution

17
EXPERIMENT NO 7
TO DETERMINE THE ORDER AND RATE CONSTANT FOR
SPONIFICATION OF ETHYL ACETATE USING CONTINUOUS
STIRRED TANK REACTOR

EQUIPMENTS USED
 Continuous stirred tank (CSTR) reactor fitted on chemical reactor service unit
 Beakers, flasks and pipette for preparing the solutions

CHEMICALS USED
 0.1 M NaOH of 0.5 L solution
 0.1 M CH3COOC2H5 of 0.5 L solution

REACTION INVOLVED
The reaction involved is the sponification of ethyl acetate.

CH3COOC2H5 + NaOH CH3COONa + C2H5OH

PROCEDURE
Prepared 0.1 molar solution of sodium hydroxide and ethyl acetate each. After that, put NaOH
solution in the CSTR. Noted the initial readings. Then put 0.1 M ethyl acetate solution in the
reagent tank. Started the peristaltic pump so that the ethyl acetate solution transfers into the
CSTR and at the same time, started the stop watch. Noted the conductivity readings after every
two minutes i-e regular interval of time.

Kept on taking the reading until the conductivity become constant. . When the conductivity
become constant, then stopped the process. Noted all the experimental data.

Then calculated the concentration at any time’t’ is given by,

Where
CA (t) = concentration at any time t
CA (0) = initial concentration
K (t) = conductivity at any time t
K (0) = initial conductivity
K (∞) = conductivity at time t=∞

18
 DETERMINATION OF ORDER AND RATE CONSTANT

Here the method used for the determination of rate constant and order is the half life
method;
According to this method;
1. Determine the concentration at each time interval and obtain a concentration
data.
2. Plot time vs. concentration data on x and y-axis respectively.
3. Draw a smooth curve among the points obtained by the time vs. concentration
data.
4. Use the half life equation as:
tf = ((0.5)1-n-1) CAo1-n
k (n-1)

OR log tf = log (((0.5)1-n-1)/ k.(n-1)) + (1-n) log(CAo)

5. Then pick CAo = 0.05, 0.04, 0.02, 0.01 and 0.006 and fill in the table (table-A) in
the calculations.
6. Next, plot log tf, vs. log CAo, and find the required slope and rate constant.

OBSERVATIONS AND CALCULATIONS

Experimental Data:

Time Conductivity Concentration

0 17.29 0.1
2 13.85 0.06969163
4 10.7 0.041938326
6 8.43 0.021938326
8 7.24 0.011453744
10 6.93 0.008722467
12 6.71 0.006784141
14 6.54 0.005286344
16 6.41 0.004140969
18 6.31 0.003259912
20 6.24 0.002643172
22 6.17 0.002026432
24 6.13 0.001674009
26 6.1 0.001409692
28 6.07 0.001145374
30 6.05 0.000969163
32 6.02 0.000704846
34 6 0.000528634
36 5.99 0.000440529
38 5.98 0.000352423

19
40 5.97 0.000264317
42 5.96 0.000176211
44 5.96 0.000176211
46 5.95 8.81057E-05
48 5.95 8.81057E-05
50 5.94 0
52 5.94 0
54 5.94 0
56 5.94 0

20
TABLE A:

CAo 0.5 CA Time required = tf Log(CAo) Log(tf)

1.2

0.8

0.6

0.4

0.2

0
0
0.05 0.025 6 – 3.6 = 2.4 -1.3 0.38
0.04 0.02 7.2 – 4.5 = 2.7 -1.3979 0.43
21
0.02 0.01 12 – 7.2 = 4.8 -1.6989 0.68
0.01 0.005 20 – 12 = 8 -2 0.903
0.006 0.003 27- 18 = 9 -2.222 0.954

22
Now, Here

slope = 1 - n = (y2 – y1)/(x2 – x1) x1 = 0 and x2 = - 2.2

= - 0.5 and y2 = 0.95
slope = 1 - n = (0.954 - 0.5) / (-2.2 – 0)

So 1 - n = - 0.7
And n = 1.7
And intercept is,
log (((0.5)1-n-1)/ k.(n-1)) = -0.7
Thus k = 4.47

Thus, rate constant = k = 4.47 and order = n = 1.7

So we have equation as,
1.7
-rA = 4.47 CA

23
Experiment no 08
TO FIND THE EFFECT OF INADEQUATE MIXING ON REACTION RATE USING
 STIRRED REACTOR WITH BAFFLE

 UNSTIRRED REACTOR WITH BAFFLE


 UNSTIRRED REACTOR WITH NO BAFFLE

EQUIPMENTS USED
 Continuous stirred tank (CSTR) reactor fitted on chemical reactor service unit
 Beakers, flasks and pipette for preparing the solutions

CHEMICALS USED
 0.1 M NaOH of 0.5 L solution
 0.1 M CH3COOC2H5 of 0.5 L solution

REACTION INVOLVED

The reaction involved is the sponification of ethyl acetate.

CH3COOC2H5 + NaOH CH3COONa + C2H5OH

PROCEDURE

CASE 1: Stirred Reactor with Baffle

Prepared 0.1 molar solution of sodium hydroxide and ethyl acetate each. After that, put NaOH
solution in the CSTR. Noted the initial readings. Then put 0.1 M ethyl acetate solution in the
reagent tank. Started the peristaltic pump so that the ethyl acetate solution transfers into the
CSTR and at the same time, start the stop watch. Note the conductivity readings after every
two minutes i-e regular interval of time.

Keep on taking the reading until the conductivity become constant. When the conductivity
becomes constant, then stopped the process. Note all the experimental data.

Then calculate the concentration at any time’t’ is given by,

24
CASE 1: OBSERVATIONS & CALCULATIONS

Time Conductivity Concentration

0 17.29 0.1
2 13.85 0.06969163
4 10.7 0.041938326
6 8.43 0.021938326
8 7.24 0.011453744
10 6.93 0.008722467
12 6.71 0.006784141
14 6.54 0.005286344
16 6.41 0.004140969
18 6.31 0.003259912
20 6.24 0.002643172
22 6.17 0.002026432
24 6.13 0.001674009
26 6.1 0.001409692
28 6.07 0.001145374
30 6.05 0.000969163
32 6.02 0.000704846
34 6 0.000528634
36 5.99 0.000440529
38 5.98 0.000352423
40 5.97 0.000264317
42 5.96 0.000176211
44 5.96 0.000176211
46 5.95 8.81057E-05
48 5.95 8.81057E-05
50 5.94 0
52 5.94 0
54 5.94 0
56 5.94 0

25
CASE 1: DETERMINATION OF REACTION RATE AT ANY TIME ‘t’:

To determine the reaction rate at any time ‘t’

1. Drawn the graph among time vs. concentration data and draw a smooth curve.
2. Selected three time intervals i-e t= 12, 14 and 16 minutes.
3. Then drawn tangents among concentrations at these time intervals.
4. These tangents represent the rate of reactions at these time intervals.

Time(min) CA rA -rA
12 0.006784141 (0.017 - 0)/(0 - 19.5) = -8.72*10-4 8.72*10-4
14 0.005286344 (0.0142 - 0)/(0 - 22) = -6.45*10-4 6.45*10-4
16 0.004140969 (0.012 - 0)/(0 - 24) = -5*10-4 5.0*10-4

26
CASE 2: UnStirred Reactor with Baffle
Repeated the same procedure as for case1, but in this case did not switch on the stirrer.
Performed the experiment without stirrer and with baffle.

CASE 2: OBSERVATIONS & CALCULATIONS

Time Conductivity Concentration

0 19.67 0.1
2 17.47 0.082567353
4 12 0.039223455
6 9.43 0.018858954
8 8.33 0.010142631
10 7.93 0.006973059
12 7.68 0.004992076
14 7.48 0.00340729
16 7.35 0.002377179
18 7.26 0.001664025
20 7.2 0.00118859
22 7.16 0.000871632
24 7.13 0.000633914
26 7.11 0.000475436
28 7.1 0.000396197
30 7.1 0.000396197
32 7.09 0.000316957
34 7.09 0.000316957
36 7.08 0.000237718
38 7.07 0.000158479
40 7.06 7.92393E-05
42 7.05 0
44 7.05 0

27
CASE 2: DETERMINATION OF REACTION RATE AT ANY TIME ‘t’:

To determine the reaction rate at any time ‘t’

1. Repeated the same procedure as for CASE 1.
2. Drawn the graph among time vs. concentration data and draw a smooth curve.
3. Selected three time intervals i-e t= 12, 14 and 16 minutes.
4. Then drawn tangents among concentrations at these time intervals.
5. These tangents represent the rate of reactions at these time intervals.

Time(min) CA rA -rA
12 0.004992076 (0.015 - 0)/(0 - 17.5) = -8.57*10-4 8.57*10-4
14 0.00340729 (0.012 - 0)/(0 – 19.2) = -6.25*10-4 6.25*10-4
16 0.002377179 (0.009 - 0)/(0 – 21.2) = -4.25*10-4 4.25*10-4

28
 CASE 3: UnStirred Reactor with No Baffle
Repeat the same procedure as for case1, but in this case did not switch on the stirrer
and removed the baffle also. Performed the experiment without stirrer and with no baffle.

CASE 3: OBSERVATIONS & CALCULATIONS

Time Conductivity Concentration

0 18.96 0.1
2 13.67 0.056674857
4 10.24 0.028583129
6 8.31 0.012776413
8 7.77 0.008353808
10 7.43 0.005569206
12 7.23 0.003931204
14 7.1 0.002866503
16 7 0.002047502
18 6.94 0.001556102
20 6.89 0.001146601
22 6.85 0.000819001
24 6.82 0.000573301
26 6.79 0.0003276
28 6.77 0.0001638
30 6.76 8.19001E-05
32 6.75 0
34 6.75 0

CASE 3: DETERMINATION OF REACTION RATE AT ANY TIME ‘t’:

To determined the reaction rate at any time ‘t’

1. Repeated the same procedure as for CASE 1 and CASE 2.

2. Drawn the graph among time vs. concentration data and draw a smooth curve.
3. Selected three time intervals i-e t= 12, 14 and 16 minutes.
4. Then drawn tangents among concentrations at these time imtervals.
5. These tangents represent the rate of reactions at these time intervals.

29
 Time(min) CA rA -rA
12 0.003931204 (0.012 - 0)/(0 - 17.4) = -6.89*10-4 6.89*10-4
14 0.002866503 (0.0095 - 0)/(0 – 19) = -5.0*10-4 5.0*10-4
16 0.002047502 (0.0071 - 0)/(0 – 21) = -3.38*10-4 3.38*10-4

CONCLUSION
From the three experiments, we have the data as

Time(min) CASE 1: -rA CASE 2: -rA CASE 3: -rA

12 8.72*10-4 8.57*10-4 6.89*10-4
14 6.45*10-4 6.25*10-4 5.0*10-4
16 5.0*10-4 4.25*10-4 3.38*10-4

RESULTS
Here it has been concluded from the results of three experiments that at all time intervals
-rA of CASE 1 > -rA of CASE 2 > -rA of CASE 3
the rate of reaction decreases.
30
EXPERIMENT NO 09
TO FIND THE EFFECT OF FLOW RATE ON REACTION RATE USING
CONTINUOUS STIRRED TANK REACTOR

EQUIPMENTS USED

 Continuous stirred tank (CSTR) reactor fitted on chemical reactor service unit
 Beakers,
 flasks and
 pipette for preparing the solutions

CHEMICALS USED

 0.1 M NaOH of 0.5 L solution

 0.1 M CH3COOC2H5 of 0.5 L solution

REACTION INVOLVED

The reaction involved is the sponification of ethyl acetate.

CH3COOC2H5 + NaOH CH3COONa + C2H5OH

PROCEDURE
Prepared 0.1 molar solution of sodium hydroxide and ethyl acetate each. After that, put
0.1 M NaOH solution in the CSTR. Noted the initial readings. Then put 0.1 M ethyl acetate
solution in the reagent tank. Sat the potentiometer speed to some value .Started the peristaltic
pump so that the ethyl acetate solution transferred into the CSTR and at the same time, started
the stop watch. Noted the conductivity readings after every two minutes i- e regular interval of
time.
Kept on taking the reading until the conductivity become constant. When the conductivity
become constant, then stopped the process. Noted all the experimental data.
Then calculated the concentration at any time’t’ is given by,

Using the design equation for CSTR

V = volume of reactant used FAo = Feed rate
xA = conversion
-rA = rate of reaction

Where
31
 FAo -rA
V= xA But FAo = CAo.V0

So -rA = (CAo.V0)(xA) / (V)

Similarly repeated the same procedure for different potentiometer speeds and
finally observed the effect of flow rate on rate of reaction.

OBSERVATIONS AND CALCULATIONS

CASE 1: When potentiometer speed set at 7

Here the flow rate V0 = 58.84 L/min (From experiment # 1)

Time Conductivity Concentration Conversion

0 17.25 0.1 0
2 16.75 0.09567474 0.043252595
4 12.73 0.060899654 0.39100346
6 10.87 0.044809689 0.551903114
8 9.32 0.031401384 0.685986159
10 8.07 0.020588235 0.794117647
12 7.05 0.011764706 0.882352941
14 6.58 0.007698962 0.923010381
16 6.38 0.005968858 0.940311419
18 6.21 0.00449827 0.955017301
20 6.07 0.003287197 0.967128028
22 5.97 0.002422145 0.975778547
24 5.88 0.001643599 0.983564014
26 5.82 0.001124567 0.988754325
28 5.74 0.000432526 0.99567474
30 5.69 0 1

Now

S.NO Time (min) Flow rate (L/min) Conversion -rA (mol/L.min)

1 10 58.84 0.794 (0.1*58.84*0.794)/(0.5) = 9.34
2 20 58.84 0.967 (0.1*58.84*0.967)/(0.5) = 11.38

32
CASE 2: When potentiometer speed set at 8

Here the flow rate V0 = 68.77 L/min (From experiment # 1)

Time Conductivity Concentration Conversion

0 17.2 0.1 0
2 15.23 0.082519965 0.174800355
4 12.52 0.058473824 0.415261757
6 10.42 0.039840284 0.601597161
8 8.78 0.025288376 0.747116238
10 7.44 0.013398403 0.866015972
12 6.97 0.009228039 0.90771961
14 6.73 0.007098492 0.929015084
16 6.53 0.005323869 0.946761313
18 6.39 0.004081633 0.959183673
20 6.27 0.003016859 0.969831411
22 6.17 0.002129547 0.978704525
24 6.09 0.001419698 0.985803017
26 6.03 0.000887311 0.991126886
28 5.97 0.000354925 0.996450754
30 5.93 0 1

Now

S.NO Time (min) Flow rate (L/min) Conversion -rA (mol/L.min)

1 10 68.77 0.866 (0.1*68.77*0.866)/(0.5) = 11.91
2 20 68.77 0.9698 (0.1*68.77*0.9698)/(0.5) = 13.3

CASE 3: When potentiometer speed set at 10

Here the flow rate V0 = 88.53 L/min (From experiment # 1)

Time Conductivity Concentration Conversion

0 16.85 0.1 0
2 13.45 0.06939694 0.306030603
4 10.46 0.042484248 0.575157516
6 8.33 0.023312331 0.766876688
8 7.16 0.012781278 0.872187219
10 6.84 0.00990099 0.900990099
12 6.59 0.007650765 0.923492349
14 6.4 0.005940594 0.940594059
16 6.25 0.004590459 0.95409541
18 6.13 0.003510351 0.96489649
20 6.04 0.00270027 0.9729973

33
 22 5.96 0.001980198 0.98019802
24 5.89 0.001350135 0.98649865
26 5.83 0.000810081 0.99189919
28 5.78 0.000360036 0.99639964
30 5.74 0 1

Now

S.NO Time (min) Flow rate (L/min) Conversion -rA (mol/L.min)

1 10 88.53 0.901 (0.1*88.53*0.901)/(0.5) = 15.95
2 20 88.53 0.965 (0.1*88.53*0.965)/(0.5) = 17.1

CONCLUSION

From the three experiments, we have the data as

Time(min) CASE 1: -rA CASE 2: -rA CASE 3: -rA

10 9.34 11.91 15.95
20 11.38 13.33 17.1

RESULTS
Here it has been concluded from the results of three experiments that at all time intervals
-rA of CASE 1 < -rA of CASE 2 < -rA of CASE 3
By increasing flow rate, the rate of reaction increases

34
Experiment No 10
Demonstration of Tubular Reactor

DESCRIPTION

Tubular Reactor or 'plug flow' reactor is in the form of a tube wrapped in a spiral around an
acrylic former which is enclosed in a transparent tank.

Water at a controlled temperature is circulated within the tank, this maintains the reactants at
constant temperatures.

Reagents are separately piped to the reactor through quick release fittings mounted on the lid.
Reagents are pre-heated in stainless steel coils before being mixed and loaded into the reactor
coil.

BASIC CONSTRUCTION AND COMPONENTS

REACTOR VESSEL

A small scale tubular reactor having a volume of 0.4 liters is capable of

demonstrating large scale behavior.
The reactor coil is mounted in a clear acrylic vessel through which heating or
cooling medium is circulated. Length of reactor coil is 20m.

HEATING COILS

Two pre-heat coils bring the reactants up to the reaction temperature separately
before they are mixed in a Y piece after which the reaction begins.

SENSORS
35
 Performance is monitored by a conductivity sensor mounted in a flow cell at the
end of the reactor coil.

FITTINGS

Quick release fittings are used for process and service connections to enable
quick mounting and removal from the service unit.

DEMONSTRATION CAPABILITIES:

The main aim of tubular reactor is:

 Determination of the rate constant

 Determination of reaction rate constant
 Investigation of the effect of througput on conversion
 Demonstration of the temperature dependance of the reaction and the rate
constant

36
Experiment No 11

To determine the rate constant and order of reaction for

saponification of ethyl acetate using half-life method using PFR

APPARATUS
 Plug Flow Reactor

Working Principle

THEORY
One or more fluid reagents are pumped through a pipe or tube and it also consists of a sensor. The
pipes or tubes are characterized by continuous gradients of concentration in the direction of flow.

Advantages:

●High efficiency than a CSTR or the same volume

● PFR may have several pipes and they are in parallel condition.
● Both horizontal and vertical operations are common.
● They can be jacketed
● Reagents may be introduced at locations even other than the inlet.

Disadvantages:

Not economical for small batches.

Applications
● Used in chemical industries like in Haber process and processes like
distillation.
● Used in biological processes like the study of bio-film.
● It is used to measure the biodegradable dissever organic carbon
in sea water

PROCEDURE:
● Made a solution (0.1M) of NaOH and ethyl acetate
● Switched on the apparatus and calibrate it
● Poured both solutions into their inlets and set T.
● When they come constantly with each other the product will form and flow through
the tubes.
● Note the initial conductivity.
● Find concentration
● Using a half-life method to find tf.

37
DIMENSIONS:
● Reactor Dimension
● Preheat coils each total length = 1.2m, reactor coil = 0, internal dia = 4.9mm,
● reactor coil id = 5mm, total volume of coil = 0.02L, reactor coil volume = 0.41 L.

CHEMICALS:

● NaOH solution 0.1M in 0.5L

● Ethyl acetate solution of 0.1M in 0.5L

PRECAUTIONS

● Handle the apparatus carefully

● Take reading accurately

FORMULA

𝑡𝑓 = ((0.5)^1−𝑛 − 1)/𝐾(𝑛 − 1)) 𝐶𝐴𝑜^1−𝑛

log 𝑡𝑓 = log ((0.5)^1−𝑛 − 1/𝐾(𝑛 − 1)) + (1 − 𝑛) log 𝐶𝐴𝑜
,−𝑟𝐴 = 1 𝐶𝐴 1.05

GRAPH:

Graphs between CAo and log of Tf also shows indirect relation through a straight line.

The reciprocal of the rate of the reaction increases exponentially with concentration.
Hence the rate of the reaction decreases exponentially with concentration.

38
Conclusion

In this experiment a saponification reaction of ethyl acetate and sodium hydroxide was
carried out in a plug flow reactor and a change in Concentration (in terms of Electrical
Conductivity) was measured with time at room temperatures of 250C. At each
conductivity, different values of concentration were obtained. The results shown that the
rate of the reaction decreased exponentially with concentration.

39