Cre Lab Manual 18bt01035

Chemical Reaction Engineering-I
CHEMICAL REACTION ENGINEERING-I

LAB MANUAL
5th CHEMICAL (20CH502)
CHEMICAL
ENgINEERING
NAME :LATHIYA SARTHAK SURESHBHAI

BRANCH :B.TECH CHEMICAL
ENROLLMENT NO .:18BT01035
BATCH:____2018________YEAR :_2020
Chemical Engineering
School of Technology
GSFC University- Vadodara
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Chemical Engineering Dept. GSFC University-Vadodara

CERTIFICATE
This is to certify
that
Mr./Miss.____________________________
Enrollment No.___________________ of
programme B.E.- 5th SEM- CHEMICAL has
satisfactorily completed __10___ Practicals in
CHEMICAL REACTION ENGINEERING -I
(20CH502) for the term of AY 2020 - 2021.
Staff in-charge Course Coordinator

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No. NAME OF EXPERIMENT DATE PAGE SIGN REMARKS
To determine the Order of reaction and activation

1 energy of the reaction between sodium thio- 1
sulphate and HCl.
To determine the kinetics of the reaction between
ethyl acetate and sodium hydroxide of same initial
2 concentration at room temperature by the integral
6
method of analysis.
To determine the kinetics of the reaction between
ethyl acetate and sodium hydroxide of different
3 initial concentration at room temperature by the
9
integral
To measure the kinetics of a reaction between ethyl
4 acetate and sodium hydroxide under condition of 12
excess ethyl acetate at room temperature.
To determine the conversion for the given
saponification reaction between ethyl acetate and
5 sodium hydroxide in Continuous Stirred Tank
15
Reactor (CSTR) under isothermal condition.
To determine the conversion for the given
saponification reaction between ethyl acetate and
6 sodium hydroxide in a Plug Flow Reactor (PFR) at 19
fixed temperature and compare it with Continuous
Stirred Tank Reactor (CSTR).
To study the performance of combined reactors
(PFR followed by MFR) and to calculate the
7 conversion achieved by this multiple reactor
22
system.
To study the kinetic behavior of cascade of stirred
8 tank reactors and determination of “number of 25
tanks” in “tanks in series model”.
(i) To plot RTD curve for a Tubular Reactor using a
pulse tracer.
9 (ii) To determine the dispersion number (D/uL) for
30
a Tubular Reactor using a pulse tracer.
(i) To plot RTD curve for a Continuous Stirred
Tank Reactor (CSTR) using a pulse tracer.
(ii) To determine the dispersion number (D/uL) for
10 a Continuous Stirred Tank Reactor (CSTR)
35
using a pulse tracer.
i) To plot RTD curve for a Packed Bed Reactor

using a pulse tracer.
11 (ii) To determine the dispersion number (D/uL) for 40
a Packed Bed Reactor using a pulse tracer.
3
INDEX
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EXPERIMENT NO-1 Date: _________

AIM: -To determine the Order of reaction and activation energy of the reaction
between sodium thio-sulphate and HCl.
APPARATUS: - 1. Glass beaker

2. Thermometer
3. Stop watch
4. 100 ml measuring Cylinder
5. Paper
CHEMICALS: -
1. 0.1 N Na2S2O3 .5H2O

2. 1N HCl solution
THEORY:-
The reaction between sodium thio-sulphate and HCl is given by,
Na2S2O3 .5H2O + 2HCl → 2NaCl + 6H2O + SO2 + S
which precipitates sulfur.
The rate of reaction of sodium thiosulfate is given by,
Keeping HCl concentration constant, the product of rate constant and HCl becomes constant
k1 and thus rate now becomes concentration of sodium thiosulfate.
Taking log on both side,
Here plot of log(rate) versus log(thiosulfate) will give straight line and slope will give order
4
of thiosulfate.
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Similarly keeping sodium thiosulfate concentration constant and changing HCl concentration,
we can find order of HCl.
For many reaction and particularly elementary reactions, the rate expression can be written as
a product of temperature dependent term & a composition dependent term as
Y = F1 (Temperature) x F2 (Composition)
= K x F2 (Composition)
For such reaction the temperature dependent term, the reaction rate constant was found in
particularly all cases to be well represented by Arrhenius law :
K = K0 e(-E/RT)
Where K0 is called the frequency factor and E is the activation energy of the reaction. Thus
expression fits experimental data well over the temperature ranges and it strongly suggest
from various points as being a very good approximation to the true temperature dependency.
The temperature dependency of the reaction is determined by the activation energy and
temperature level as shown by curve of ln K Vs 1/T. These finding can be summarized as:
1. From Arrhenius law, plot of lnK Vs 1/T gives a straight line with large slope for a
large E and small slope for small E.
2. Reaction with high activation energy is very temperature sensitive, reaction with low
activation energies are relatively temperature sensitive.
3. For the Arrhenius law, the frequency factor K0 does not affect the temperature
sensitivity of a reaction.
At same concentration but different temperature, Arrhenius law is given by
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From this equation, activation energy also can be determined.

PROCEDURE:-
1. Prepare 250 ml of 0.1 N sodium thiosulfate and 250 ml of 1 M HCl solution.

2. Take 250 ml clean beaker and fill 50 ml of 0.1 N sodium thiosulfate solution.
3. Keep the beaker containing sodium thio-sulphate on a paper on which a cross mark
was made.
4. The 10 ml HCl (1 M) solution is poured in beaker and then the beaker was stirred.
Simultaneously the stop watch is started.
5. The time when the cross sign ceased to be invisible due to formation of sulphur
precipitates is noted.
6. Similarly follow the same procedure for the other concentration of sodium thio-
sulphate by keeping HCl volume and concentration constant.
7. Follow the same procedure by changing HCl concentration and keeping sodium
thiosulfate volume and concentration constant.
8. Repeated the same procedure for a different steady state temperature (set temperature
interval 5 °C) and a graph of ln K Vs 1/T is plotted.
GRAPH: - (i) Plot a graph of log(rate) versus log(thiosulfate) & determine the order of
reaction of thiosulfate. The nature of graph is a straight line.
(ii) Plot a graph of log(rate) versus log(HCl) & determine the order of reaction of HCl. The
nature of graph is a straight line.
(iii) Plot a graph of ln K Vs 1/T.
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OBSERVATION TABLES: -
Table 1
No Volume Volume Concentr Volume of 1 Time Rate Log(r Log(Co

. of of water ation of M HCl (ml) taken to (M/s) ate) ncentr
sodium sodium cross ation of
thiosulfa (ml) thiosulfat become Initial sodium
te e (M) s conc of thiosulf
invisible S.T/time ate)
(ml) (s)
1 50 0 0.1 10 25.6 0.0039 -5.54 -2.3
2 40 10 0.08 10 31.7 0.00315 -5.76 -2.52
3 30 20 0.06 10 43.1 0.00232 -6.06 -2.81
4 20 30 0.04 10 70.85 0.00141 -6.56 -3.218
5 10 40 0.02 10 222 0.00045 -7.7 -3.91
Table 2
No Volume of Volume Volume Concentrat Time Rate Log(r Log(Co

. 0.2 M of of HCl ion of HCl taken to (M/s), ate) ncentr
sodium water (ml) (M) cross Initial ation
thiosulfate becomes conc of of HCl)
(ml) invisible S.T/ti
(ml) (s) me
1 10 0 50 1 155 0.006 -5.025 0
2 10 10 40 0.8 158 0.006 -5.029 -0.22
3 10 20 30 0.6 152 0.006 -5.02 -0.51
4 10 30 20 0.4 170 0.0058 -5.14 -0.91
5 10 40 10 0.2 156 0.006 -5.026 -1.6

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Table 3

Sr Temperatur Concentration Volume Time taken Rate Rate

No e (C) of Sodium of 1 M to cross (M/s) constant
thiosulfate HCl becomes (K)
invisible (s)
1 32 0.1 10 25.63 0.0039
2 40 0.1 10 14.56 0.00686
CALCULATION: -
1 Slope of graph of log(rate) versus log(thiosulfate) = ____1_____
2 Slope of graph of log(rate) versus log(HCl) = _____0_____
3 Activation Energy E = _____56.025______J/mol
For Table 1
Rate = k CAn CBm
Where, A = Sodium thiosulfate
B = HCl
As volume of HCl is constant, m = 0
So, Rate = k CAn CBm = k’ CAn
Taking log on both side, we get,
ln(rate) = ln(k) + n ln CA
Now, on plotting graph, we get,
log(Rate) versus log(Concentration of Sodium thiosulfate)

0
-2.3 -2.52 -2.81 -3.22 -3.91
-1
-2
-3
-4
-5
-6
-7
-8
-9
8
On solving,
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Slope = 1.341195371
Intercept = -2.365327744
For Table 2
Similarly,
Rate = k CAn CBm
Where, A = Sodium thiosulfate
B = HCl
As volume of Sodium thiosulfate is constant, n = 0
So, Rate = k CAn CBm = k’ CBm
Taking log on both side, we get,
ln(rate) = ln(k) + m ln CB
Now, on plotting graph, we get,
log(Rate) versus log(Concentration of HCl)

0
-5.03 -5.03 -5.02 -5.14 -5.03
-0.2
-0.4
-0.6
-0.8
-1
-1.2
-1.4
-1.6
-1.8
On solving,
Slope = 0.01882185
Intercept = -5.035803441
For Table 3
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We know that, Arrhenius law is given as

(Rate)2 / (Rate)1 = (E/R) (1/T1 – 1/T2)
On putting values from table 3, we get,
(0.00686/ 0.0039) = (E/8.314) (1/305 – 1/313)
On solving for E,
E = 56.025 kJ/ mol
RESULT: -
1. Activation energy of the reaction between sodium thio-sulphate and HCl

using the Arrhenius law is found to be _____56.025_____J/mol.
2. Order of reaction between sodium thio-sulphate and HCl is found to
be__1__with respect to sodium thio-sulphate and ___0___ with respect to
HCl .
CONCLLUSION: -
REMARK:
SIGN:

AIM: - To determine the kinetics of the reaction between ethyl acetate and sodium
10
hydroxide of same initial concentration at room temperature by the integral method of

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analysis.

APPARATUS: -
1. 500 ml beaker
2. Stop watch
3. 100 ml conical flask
4. Batch reactor
CHEMICALS: -
1. Ethyl acetate
2. NaOH
3. HCl
4. Phenolphthalein
THEORY:-
The reaction between NaOH and Ethyl acetate is given by,
NaOH + CH3COOC2H5 → CH3COONa + C2H5OH
In the integral method of analysis, the order of reaction under consideration assumed and the
integral rate expression is subsequently obtained on based on this suitable graph is drawn by
using the experimental data which reveals the fitness of such data. If the fit is satisfactory
then the assumed order is correct, otherwise a different order is assumed and the same
method is continued until a satisfactory it is obtained. It is also possible to calculate from the
graph the rate constant, thus the kinetics of a specified temp can be determined.
PROCEDURE:-
1. Standardize NaOH and HCL solutions.

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2. Take 500 ml of NaOH solution of 0.1 N in a batch reactor and

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start stirrer.

3. To this, add 500 mal of 0.1 N Ethyl Acetate and start stop
watch.
4. Take out 10 ml sample from the reactor at every one minute
and pour into the beaker already containing 0.1 N, 10 ml HCl.
5. Add phenolphthalein into the sample and titrate against 0.1 N
NaOH.
6. Find NaOH concentration against time.
7. Measure reaction temperature.
8. Do necessary calculations.
OBSERVATIONS: -
Reaction temperature : 30 degree C
1) Normality of NaOH solution (N3) = 0.1N

2) Normality of Ethyl acetate solution = 0.1N
3) Normality of HCL solution (N1)= 0.1 N
4) Volume of HCL solution (V1)= 10 ml
5) Volume of NaOH (V3) in burette
6) Volume of sample (V2) = 10 ml
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OBSERVATION TABLE: -
Sr. No. Time (t), Concentration of (1/CA)

min NaOH, (CA)
(1) 2 0.043 23.25
(2) 4 0.031 32.25
(3) 6 0.027 37.03
(4) 8 0.025 40
(5) 10 0.023 43.47
(6) 12 0.023 38.46
(7) 14 0.027 37.03
(8) 16 0.02 50
CALCULATIONS:
CA = N2 = (N1V1-N3V3)/V2
GRAPH:
Plot (1/CA) vs. t .Intercept will give 1/CA0 and slope will give rate constant k.
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60
50
40
30
20
10
0
2 4 6 8 10 12 14 16
Y 2−Y 1
Slope K = = 2.5
X 2−X 1
RESULT: -
1. The order of reaction was found to be – 2nd Order

2. Rate constant k = 2.5
CONCLLUSION: - After carrying out the experiment, the rate equation becomes
–rA= 2.5 CACB , where the rate constant k = 2.5 and the overall order of reaction is 2.
REMARK
SIGN
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AIM: - To determine the kinetics of the reaction between ethyl acetate and sodium
hydroxide of same initial concentration at room temperature by the integral method of
analysis.
APPARATUS: -
5. 500 ml beaker
6. Stop watch
7. 100 ml conical flask
8. Batch reactor
CHEMICALS: -
5. Ethyl acetate
6. NaOH
7. HCl
8. Phenolphthalein
THEORY:-
The reaction between NaOH and Ethyl acetate is given by,
NaOH + CH3COOC2H5 → CH3COONa + C2H5OH
In the integral method of analysis, the order of reaction under consideration assumed and the
integral rate expression is subsequently obtained on based on this suitable graph is drawn by
using the experimental data which reveals the fitness of such data. If the fit is satisfactory
then the assumed order is correct, otherwise a different order is assumed and the same
method is continued until a satisfactory it is obtained. It is also possible to calculate from the
graph the rate constant, thus the kinetics of a specified temp can be determined.
15
PROCEDURE:-
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2. Take 500 ml of NaOH solution of 0.1 N in a batch reactor and
start stirrer.
3. To this, add 500 mal of 0.1 N Ethyl Acetate and start stop
watch.
4. Take out 10 ml sample from the reactor at every one minute
and pour into the beaker already containing 0.1 N, 10 ml HCl.
5. Add phenolphthalein into the sample and titrate against 0.1 N
NaOH.
7. Measure reaction temperature.
OBSERVATIONS: -
Reaction temperature : 29 degree C

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Sr. No. Time (t), Concentration of XA =1- CA/CA0 ln( M – XA /M(1-XA))

min NaOH, (CA)
(1) 2 0.022 0.56 0.492
(2) 4 0.02 0.6 0.559
(3) 6 0.0175 0.65 0.657
(4) 8 0.0155 0.69 0.748
(5) 10 0.015 0.7 0.773
(6) 12 0.013 0.74 0.885
(7) 14 0.015 0.7 0.773
(8) 16 0.014 0.72 0.827
9 18 0.0125 0.75 0.916
CALCULATIONS:
M = CBO / CAO
= 0.1/0.05
M=2
NOW,
CA = N2 = (N1V1-N3V3)/V2
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GRAPH:
Plot ( ln (M – XA / M(1-XA)) vs. t . Slope will give rate constant k.
Y 2−Y 1 Slope K =
X 2−X 1
= 0.0239
RESULT: -
3. The order of reaction was found to be – 2nd Order

4. Rate constant k = 0.0239
CONCLLUSION: - After carrying out the experiment, the rate equation becomes
–rA= 0.0239CACB , where the rate constant k = 0.0239 and the overall order of reaction is 2.
REMARK
SIGN
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EXPERIMENT NO- 4 Date: _15/12/2020___
AIM: - To measure the kinetics of a reaction between ethyl acetate and sodium
hydroxide under condition of excess ethyl acetate at room temperature.
APPARATUS: -
- 500 ml beaker
- Stop watch
- 100 ml conical flask
- Batch reactor
CHEMICALS: -
- Ethyl acetate
- NaOH
- HCl
- Phenolphthalein
THEORY:-
Under normal conditions, reactions between ethyl acetate and NaOH is of second order.
However if concentration of one of the reactants is in excess it remains constant through the
reaction. Hence the above reaction is a pseudo first order reaction and a apparently a first
order reaction. This fact is verified by this experiment.
PROCEDURE:-

2. Take 500 ml of NaOH solution of 0.1 N in a batch reactor and start stirrer.
3. To this, add 500 mal of 0.3 N Ethyl Acetate and start stop watch.
4. Take out 10 ml sample from the reactor at every one minute and pour into the
beaker already containing 0.1 N, 10 ml HCl.
5. Add phenolphthalein into the sample and titrate against 0.1 N NaOH.
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OBSERVATIONS: -
Reaction temperature : __31°C______

3) Normality of HCL solution (N1)= 0.5N
No. Time (t) CA ln

in min
(CA0/CA)
1. 1 0.021 0.112
2. 2 0.0178 0.2778
3. 3 0.0141 0.5087
4. 4 0.0133 0.569
5. 5 0.0122 0.655
6. 6 0.011 0.759
7. 7 0.0102 0.8346
CALCULATION: -
CA = N2 = (N1V1-N3V3)/V2
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Graph: - ln (CA/CA0) Vs time t

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If the straight line passes through the origin then the slope gives the rate of reaction.

0.9
0.83
0.8
0.76
0.7
0.66
0.6
0.57
0.5 0.51
0.4
0.3
0.28
0.2
0.1 0.11
0
0 1 2 3 4 5 6 7 8
RESULT: -
 The value of the rate constant of pseudo first order reaction is = 0.13(1/min)
 Nature of graph: _straight line passing through origin -rA=0.13cA¹
CONCLLUSION: -
From the above experiment we can conclude that the nature of graph is a straight line passing
through origin.
REMARK
SIGN
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EXPERIMENT NO-5 Date: ________

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AIM: To determine the conversion for the given saponification reaction between ethyl
acetate and sodium hydroxide in Continuous Stirred Tank Reactor (CSTR) under
isothermal condition.
APPARATUS: -
1.500 ml Glass beaker
2.100 ml Conical flask
3. Stop watch
4. CSTR
CHEMICALS: -
1. Ethyl acetate
2. NaOH
3. HCl
4. Phenolphthalein
THEORY:
In an ideal CSTR (that is an ideal steady state flow reactor) the contents in the reactor are
well mixed and have uniform composition throughout. Thus the exit stream has the same
composition as the fluid within the reactor. This type of reactor is also known as MIXED
FLOW REACTOR.
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Reactor volume (volume of fluid in the reactor) = VR, Liters,

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Volumetric feed rate (volumetric feed rate of A + volumetric feed rate of B) =V0 , LPM Space
time = τ = VR / Vo, min
The performance equation for the CSTR at steady state is
V R C A 0 X A C A 0−C A
τ= = =
V0 −r A −r A
XA & rA are evaluated at exit stream conditions, which are the same as the conditions within
the reactor.
For a second order reaction:
A+B C+D
With CAO = CBO and negligible change in density of reaction mixture
The reaction rate (rate of disappearance of A),

- rA = k CA2
HENCE
V R C A 0 X A C A 0−C A
τ= = =
V0 −r A k C A2
Degree of conversion, XA = (CAo - CA) / CAo
and rate of reaction, -rA = CAo XA / τ , gmol/l-min
2
the rate constant, k = (CAO- CA ) / (τ CA ) , l/gmol-min
PROCEDURE:-
1. First of all check that all the valves (on air and water line) are in closed position.
2. Switch ON the air compressor and allow it to run till it is fully loaded.(0.5 kg/ cm 2 of air
which is needed in the experiment)
3. Adjust the flow rate of the reactants from the storage tanks to about 20 LPH and allow the
reactants into the CSTR at this prefixed value by the compressed air.
4. Switch on the stirrer and maintain a suitable speed so as not to vigorously agitate the liquid
in the reactor.
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5. When the reaction mixture starts overflowing, start collecting samples of 10 ml pour into
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the beaker already contained 0.1 N, 10 ml HCl.

7. Keep on collecting the sample until steady state is attained. i.e. the composition of the last
two samples has the same value.
OBSERVATIONS: -
Reaction temperature : _____30 C___

7) Volume of CSTR = 2.19 Litre
8) Volumetric Flow rate of NaOH and Ethyl acetate = _15__LPH NaOH + _15__LPH Ethyl
acetate.
9) Space time ( τ)= V/ V0 = 2.19/30=0.073hr.
where V = Volume of reactor
V0 = Volumetric flow rate of NaOH
Sr. Space Tempera Concent

No. Time, hr ture (̊C) ration of XA
( τ) NaOH,
(CA)
1. 0.073 30 0.031 38%
2. 0.0438 30 0.035 30%
CALCULATIONS:
CA = N2 = (N1V1-N3V3)/V2
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 CA = N2 = (N1V1-N3V3)/V2
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=0.1*10-0.1*6.5/10=0.035
 CA = N2 = (N1V1-N3V3)/V2
=0.1*10-0.1*6.9/10=.031
 XA =1-CA/CAO=1-0.031/0.05=.38=38%
 XA =1-CA/CAO =1-.035/0.05=.30=30%
RESULT: -
1. The conversion of reaction between NaOH and Ethyl Acetate at _30___̊C is found to be
___38__% at __0.073__ space time CSTR.
CONCLLUSION: -
25
EXPERIMENT NO-6 Date: 16 Dec.

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2020

AIM: To determine the conversion for the given saponification reaction between ethyl
acetate and sodium hydroxide in a Tubular Flow Reactor at fixed temperature
APPARATUS: -
2.100 ml conical flask
3. Stop watch
4. Tubular reactor
CHEMICALS: -
1. Ethyl acetate
2. NaOH
3. HCl
4. Phenolphthalein
THEORY:
The first of the two ideal steady-state flow reactors is variously known as the plug flow, slug
flow, piston flow, ideal tubular, and unmixed flow reactor. It can be referred as the plug flow
reactor, or PFR, and to this pattern of flow as plug flow. It is characterized by the fact that the
flow of fluid through the reactor is orderly with no element of fluid overtaking or mixing with
any other element ahead or behind. Actually, there may be lateral mixing of fluid in a plug
flow reactor; however, there must be no mixing or diffusion along the flow path. The
necessary and sufficient condition for plug flow is for the residence time in the reactor to be
the same for all elements of fluid.
Reactor volume (volume of fluid in the reactor) = VR, Liters,
Volumetric feed rate (volumetric feed rate of A + volumetric feed rate of B) =V0 , LPM Space
time = τ = VR / Vo, min
The performance equation for the PFR at steady state is

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For a second order reaction:
A+B C+D
With CAO = CBO and negligible change in density of reaction mixture
PROCEDURE:-
1. First of all check that all the valves (on air and water line) are in closed position.
2. Switch ON the air compressor and allow it to run till it is fully loaded.
3. Adjust the flow rate of the reactants from the storage tanks and allow the reactants into the
tubular at this prefixed value by the compressed air.
4. When the reaction mixture leaves from the outlet, start collecting samples of 10 ml pour
into the beaker already contained 0.1 N, 10 ml HCl.
6. Keep on collecting the sample until steady state is attained. i.e. the composition of the last
two samples has the same value.
7. Measure the reaction temperature.
OBSERVATIONS: -
Reaction temperature : 30·c
1) Normality of NaOH solution (N3) = 0.055 N

2) Normality of Ethyl acetate solution = 0.05 N
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7) Length of reactor = 9800 mm approx.
8) Diameter of reactor = 10 mm
9) Volume of tubular reactor = 0.77 Liter
10) 1.Volumetric Flow rate of NaOH and Ethyl acetate = _30__LPH NaOH + _30__LPH
Ethyl acetate
2. Volumetric Flow rate of NaOH and Ethyl acetate = _20__LPH NaOH + _20__LPH Ethyl
acetate
11) Space time ( τ)= V/ V0
Where V = Volume of reactor
V0 = Volumetric flow rate of NaOH
Sr. Space Tempera Concentr

No. Time ture (̊C) ation of XA = 1-
( τ) NaOH, Ca/CA0
(CA)
1. 0.0128 30 0.0417 24
2. 0.019 30 0.0395 28
CALCULATIONS:
CA = N2 = (N1V1-N3V3)/V2
For 1. Space time ( τ)= V/ V0 = 0.77/ 60 = 0.0128
XA = 1-Ca/CA0 = 1- 0.417 / 0.055 = 24 %
2. Space time ( τ)= V/ V0 = 0.77 / 40 = 0.019
XA = 1-Ca/CA0 = 1- 0.395 / 0.055 = 28%

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RESULT: -

1. The conversion of reaction between NaOH and Ethyl Acetate at 30C is found to be
__24___% at _0.0128 hr___ space time in a Tubular Reactor.
2. The conversion of reaction between NaOH and Ethyl Acetate at _30___C is found to be
__28___% at _0.019hr___ space time in a Tubular Reactor.
CONCLUSION: -
By reducing volumetric flow rate so, space time is increase so it means that it will spend
more time to process in reactor so conversion is increase.
REMARK:-
Increasing space time by reducing molar flow rate
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AIM: TO Study the kinetic behavior of cascade of stirred tank reactors and
determination of “number of tanks” in “tanks in series model”.
APPARATUS: -
2.100 ml Conical flask
3. Stop watch
4. CSTR in series
CHEMICALS: -
1. Ethyl acetate
2. NaOH
3. HCl
4. Phenolphthalein
THEORY:
Consider a system of N mixed reactors connected in series. Though the concentration is

uniform in each reactor, there is nevertheless a change in concentration as fluid moves from
reactor to reactor. This stepwise drop in concentration, suggests that larger the number of
units in series the closer should the behavior of the system approach the plug flow.
Let us now quantitatively evaluate the number of units in series of N equal-size mixed
reactors. Density changes are assumed to be negligible; hence ε = 0 and t = T. As a rule with
mixed reactors it is more convenient to develop the necessary equation in terms of
concentration rather than fractional conversion; therefore we also use this approach. The
nomenclature used is shown in figure with subscript I referring to the i th vessel.
A first order reaction with no volume change is to be carried out in three CSTR placed in
series. The effluent concentration of A from the reactor 1 is
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CA1 = CA0 / (1 + τ1* k1) (1)

From a material balance on reactor 2,
V2 = (FA1 – FA2) / - rA2 = vo (CA1 – CA2) / k2 CA2 (2)
Solving for CA2 the concentration exiting the second reactor, we get
CA2 =CA1/ (1+T2 * k2) = CAO/ (1 + T1 * k1)* (1 + T2*k2) (3)
Material balance on reactor 3
V3 = FA2 – FA3 / (- rA3) = vo (CA2 - CA1) / k3 CA3 (4)
Solving for CA3, the concentration exiting the third reactor, we get
CA3= CA2 \ (1 +τ3* k3) = CAO / [(1 +τ1*k1)*(1 +τ2*k2)*(1 + τ3 *k3)] (5)
If instead of three such cstr in series if we have n equal size cstr connected in series (τ 1= τ2= τ3
= ----- = τn = τ) operating at the same temperature (k 1 = k2 =------ kn= k) the concentration
leaving the last reactor would be
CAn = CAo / (1 + τ k)n (6)
The conversion for these n tank reactors in series would be,
X = 1 – [1\ (1 + T* k) n] (7)
A plot of the conversion as a function of the number of the reactors in series for a first order
reaction is shown in figure. For various value of the damkohler number (T*k), observe from
figure that when the product of the space time and the specific reaction rate is relatively large,
31
Page

say, Da>1 approximately 90% conversion is achieved in two or three reactors; thus the cost
of adding subsequent reactors might not be justified. When the product of T & k is small,
Da< 0.1 the conversion continues to increases significantly with each reactor added.
PROCEDURE:
1. Adjust the flow rate of the reactants from the storage tanks to about 10 LPH and allow
the reactant into the cascade of the stirred reactor at this prefixed value.
2. Switch on the stirrer and maintain a suitable speed so as not to vigorously agitate the
liquid in the reactor.
3. When the reaction starts overflowing, start collecting the samples of 10 ml from each
of the reactors
4. Pipette out 10 ml reaction mixture from each reactor and transfer into the flask
containing 10 ml 0.1 N HCl.
5. Titrate the contents with NaOH using phenolphthalein indicator
6. Keep on the collecting the sample until the steady state is attained. i.e. the composition
of the last two samples has the same value.
7. Do necessary Calculations.
OBSERVATIONS:
Room temperature : 31
1) Normality of NaOH solution (N3) = 0.05 N

2) Normality of Ethyl acetate solution = 0.05 N
7) Volume of each CSTR = 2.4 Litre
8) Volumetric Flow rate of NaOH and Ethyl acetate = 15 LPH NaOH + 15 LPH Ethyl
acetate
9) Total volumetric flow rate V0 = 30 LPH

32
Page

OBSERVATION TABLE:
FOR CSTR -1
Sr. Vol. of sample taken Conc. of Conversion

No. NaOH
(V1) (ml) (XA1)
1 10 0.015 0.4
FOR CSTR -2
Sr. Vol. of sample taken Conc. of Conversion

No. NaOH
(V1) (ml) (XA1)
1 9.9 0.0131 0.47
FOR CSTR -3
Sr. Vol. of sample taken Conc. of Conver

No. NaOH sion
(V1) (ml)
(XA1)
1 9.2 0.0097 0.61
CALCULATION:
For CSTR 1
33
Xa = 1 – CA/CAO
Page
= 1 – 0.015/0.025

= 0.4
For CSTR 2
Xa = 1 – CA/ CAO
= 1 – 0.0131/ 0.025
= 0.47
For CSTR 3
Xa = 1 – CA/ CAO
= 1 – 0.0097/ 0.025
= 0.61
RESULT:
CONCLUSION:
34
EXPERIMENT NO-8
Page

Date: 24TH OCT 2020
AIM: (i) To plot RTD curve for a Tubular Reactor using a pulse tracer.
(ii) To determine the dispersion number (D/uL) for a Tubular Reactor using a
pulse tracer.
APPARATUS:
 Tubular Reactor
 Titration set
 Air compressor
CHEMICAL:-
• HCl
• Water
 NaOH
 Phenolphthalein
THEORY:
The three basic reactor models viz., batch, back mix (CSTR) and PFR are based on ideal
concepts. We often apply these models to determine the conversion and other parameters.
However, owing to non-ideality prevalent in the 'real' systems, the conversion obtained may
not be the true conversion. How do we account for this non-ideality? The residence time
distribution (RTD) or more precisely the E(t) function may be looked upon as a correction
factor to account for the non-ideality. The causes of non-ideality could be channeling and
back mixing in the case of a PFR and dead zones and non-uniform mixing in the case of a
CSTR.
Imagine that 10 atoms are injected in a PFR in a short time. Since, there is no axial mixing in
the PFR, ideally all these atoms should come out of the reactor at the same time. However,
this is not the case with the real system. Different atoms take different time to come out of the
reactor. The time the atoms have spent in the reactor is called the residence time and the
distribution of the various atoms coming out the reactor with respect to time is called the
residence time distribution. RTD can be determined experimentally by injecting an inert
chemical, molecule, or atom, called tracer, into the reactor at some time t=0 and then
measuring the tracer concentration 'C' in the exit stream as a function of time. Pulse and step
35
inputs are the two commonly used methods of injection.

 Pulse Input
Page

In a pulse input, an amount of tracer No is suddenly injected in one shot into the feed stream
entering the reactor in as short time as possible. The outlet concentration is then measured as
a function of time. The effluent concentration-time curve is referred to as the C curve in the
RTD analysis. If we select an increment of time ∆t sufficiently small that the concentration of
tracer, C(t), exiting between time t and t+∆t is essentially constant, then the amount of tracer
material, ∆N, leaving the reactor between time t and t + ∆t is
where, v is the effluent volumetric flow rate. In other words, ∆N is the amount of material
that has spent an amount of time between t and t + ∆t in the reactor. If we now divide by the
total amount of material that was injected into the reactor, N0, we obtain
which, represents the fraction of the material that has a residence time in the reactor between
time t and t + ∆t.
For a pulse injection we define
so that
This quantity E(t) is called the residence time distribution function. It describes in a
quantitative manner how much time different fluid elements have spent in the reactor.
Re-writing the above equations in the differential form,
dN= vC(t)dt
and integrating, we obtain
The volumetric flow rate v is constant, and so we can define E(t) as:
The integral in the denominator is the area under the C curve.

36
Page

As is the case with other variables described by distribution functions, the mean value of the
variable is equal to the first moment of the RTD function, E(t). Thus the mean residence time
is
It is very common to compare RTDs by using their moments instead of trying to compare
their entire distributions. For this purpose, moment commonly used is taken about the mean
and is called the variance, or square of the standard deviation. It is defined by
The Dispersion number is defined as D/uL and is given by:
PROCEDURE:-
1. Start the flow of water (around 60 LPH) in the Tubular Reactor and achieve steady state.
2. Take 10 ml of 1N NaOH in a syringe and inject it near the inlet of reactor
3. Withdraw the sample at regular interval of time ( 5 sec) and titrate it against std. 0.1N HCl.
4. Take around 10 readings
5. Determine concentration of each samples
6. Plot graph of C(t) Vs time ,E(t) Vs time ,t.E(t) Vs time and (t-t m2).E(t) vs time using the
readings of observation table and calculate area under the curve of each graph.
7. Find dispersion number
37
Page
OBSERVATIONS: -

1. Initial Normality of NaOH =1 N (10 ml)

2. Normality of HCl = 0.1 N
3. Volume of sample taken =10 ml
OBSERVATION TABLE:
Sr Time Burette Concn of E(t) tE(t) (t-tm)2 (t- tm)2E(t)

No (t) reading NaOH
(ml)
1 30 0.1 0.001 0.00158 0.03 0.9 0.001422
2 35 0.2 0.002 0.00317 0.07 2.45 0.007767
3 40 5.9 0.059 0.0936 2.36 94.4 8.83584
4 45 4.3 0.043 0.06825 1.935 87.015 5.938774
5 50 1.2 0.012 0.019 0.6 30 0.57
6 55 0.5 0.005 0.00793 0.275 15.1 0.119743
7 60 0.2 0.002 0.00317 0.12 7.2 0.022824
8 65 0.1 0.001 0.00158 0.065 4.225 0.006676
9 70 0.1 0.001 0.00158 0.070 4.9 0.007742
10 75 0.1 0.001 0.00158 0.075 5.625 0.008888
CALCULATIONS:-
1. Concentration of NaOH, C(t)

N1V1 = N2V2
N2V 2
N 1=
V1
= 0.1*0.1/10
= 0.001 N
2. Residence time distribution Function,
0.001
=
0.127
=0.007874
3. Mean residence time,

38
Page

5.6
¿
0.127
= 44.09 sec
4. Variance,
251.9
= – (44.09)2
0.127
= 39.5
5. Dispersion Number (D/uL),
GRAPHS:
39
Page

40
Page

RESULT:-
Concentration of NaOH, C(t) = 0.001 N
Residence time distribution Function (RTD)= 0.007874
41
Page

AIM: (i) To plot RTD curve for a Continuous Stirred Tank Reactor (CSTR) using a
pulse tracer.
(ii) To determine the dispersion number (D/uL) for a Continuous Stirred Tank
Reactor (CSTR) using a pulse tracer.
APPARATUS:
 CSTR
 Titration set
 Air compressor
CHEMICAL:-
• HCl
• Water
 NaOH
 Phenolphthalein
THEORY:
CSTR.
42

Page

 Pulse Input
so that
dN = vC(t)dt
43

Page

is
PROCEDURE:-
1. Start the flow of water in the CSTR (around 1 LPM) and achieve steady state.
2. Take 10 ml of 5N NaOH in a syringe and inject it near the inlet of reactor and take zero
reading
3. Withdraw the sample at regular interval of time (15 sec) and titrate it against std. 0.1N HCl
4. Take around 10-15 readings
5. determine concentration of each sample
7. Find dispersion number
44
Page

OBSERVATIONS: -
1 Initial Normality of NaOH = 5 N
2 Normality of HCl = 0.1 N
3 Volume of sample taken =10 ml
OBSERVATION TABLE:
Sr Time (t) Burette Concn of E(t) tE(t) (t-tm)2 (t- tm)2E(t)

No reading (ml) NaOH
1 0 4 0.04 0.0123 0 15876 195.27
2 30 1.9 0.019 0.0058 0.174 9216 53.45
3 60 1 0.01 0.0030 0.18 4356 13.068
4 120 1 0.01 0.0030 0.36 36 0.108
5 180 0.6 0.006 0.0018 0.324 2916 5.2488
6 240 0.4 0.004 0.0012 0.288 12996 15.5952
7 300 0.3 0.003 0.00092 0.27 30276 27.85
8 360 0.2 0.002 0.0006 0.216 54756 32.85
9 420 0.1 0.001 0.0003 0.126 86436 25.93
10 480 0.1 0.001 0.00030 0.144 125316 37.59
11 540 0.05 0.0005 0.00015 0.081 171396 25.709
12 600 0.025 0.00025 0.00008 0.048 224676 17.79
13
14
15
CALCULATIONS:-
1. Concentration of NaOH,C(t)
N1V 1
N 2= 0.1∗4
V2 = 10 = 0.04
2. Residence time distribution Function,
= 126 sec
45
4. Variance,
Page

= 15123.1 ( sec)2
= 6.8
GRAPHS:
1 Plot the graph of C(t) v/s time
700
600
500
400
Time
300 Time
tE(t)
200
100
0
1 2 3 4 5 6 7 8 9 10 11 12
C(t)
46
2 Plot the graph of E(t) v/s time

Page

700
600
500
400
Time
300
200
100
0
1 2 3 4 5 6 7 8 9 10 11 12
E(t)
3 Plot the graph of t E(t) v/s time
700
600
500
400
Time
300
200
100
0
1 2 3 4 5 6 7 8 9 10 11 12
tE(t)
4 Plot the graph of (t-tm)2 E(t) v/s time

47
Page

700
600
500
400
Time
300
200
100
0
(t-tm)2E(t)
RESULT:-
The dispersion number (D/uL) for a Continuous Stirred Tank Reactor (CSTR) using a
pulse tracer is 6.8
CONCLUSION:-
As time increase variance (σ ¿ decrease and once time reach after that time variance will
increase as time increase. as variance changes according to that dispersion number(d/ul)
changes
EXPERIMENT NO-11 Date:29/12/2020

48
Page
AIM: (i) To plot RTD curve for a Packed Bed Reactor using a pulse tracer.

(ii) To determine the dispersion number (D/uL) for a Packed Bed Reactor using a
pulse tracer.
APPARATUS:
 Packed Bed Reactor
 Titration set
 Air compressor
CHEMICAL:-
• HCl
• Water
 NaOH
 Phenolphthalein
THEORY:
CSTR.
49
 Pulse Input
Page

so that
dN = vC(t)dt

50
Page

is
PROCEDURE:-
1. Start the flow of water in the Packed Bed Reactor to build up the liquid level and to
achieve steady state
2. Measure the steady state flow rate
3. Take 10 ml of 1N NaOH in a syringe and inject it near the inlet of reactor.
4. Withdraw the sample at regular interval of time and titrate it against std. 0.1N HCl
5. Take around 15 readings
OBSERVATIONS: -
1 Initial Normality of NaOH = 5 N
51
2 Normality of HCl = 0.1 N

Page
3 Volume of sample taken = V2= 10 ml

OBSERVATION TABLE:
Sr No Time Burette Concn of t*C(t) t^2*C E(t) t*E(t) (t-tm)2 (t- tm)2E(t)
(t) reading NaOH (t)
(ml)
1 60 10 0.1 6 360 0.00833 0.500 1958.06 16.3107
2 90 14 0.14 12.6 1134 0.01167 1.050 203.063 2.36974
3 120 8 0.08 9.6 1152 0.00667 0.800 248.063 1.65458
4 150 4 0.04 6 900 0.00333 0.500 2093.06 6.9699
5 180 3 0.03 5.4 972 0.00250 0.450 5738.06 14.3452
6 210 1 0.01 2.1 441 0.00083 0.175 11183.1 9.28194
TOTAL 0.4 41.7 4959
CALCULATIONS:-
6. Concentration of NaOH,
N1V 1
N 2=
V2
= 0.1*10/10
= 0.1 N
= 41.7/0.4
= 104.25 sec
8. Variance,
= 4959/0.4 – (104.25)^2
=12397.5 -10868.06
=1529.43 sec^2
52

Page

=0.140
GRAPHS:
4 Plot the graph of C(t) v/s time:
C(t) vs t
0.16
0.14
0.12
0.1
0.08
C(t)
0.06
0.04
0.02
0
40 60 80 100 120 140 160 180 200 220
t
5 Plot the graph of E(t) v/s time:
E(t) vs t
0.01
0.01
0.01
0.01
E(t)
0.01
0
40 60 80 100 120 140 160 180 200 220
t
53
Page

6 Plot the graph of t E(t) v/s time:
t*E(t) vs t
1.2
0.8
t*E(t)
0.6
0.4
0.2
0
40 60 80 100 120 140 160 180 200 220
t
7 Plot the graph of (t-tm)2 E(t) v/s time:
(t-tm)^2E(t) vs t
18
16
14
12
(t-tm)^2E(t)
10
8
6
4
2
0
40 60 80 100 120 140 160 180 200 220
t
RESULT:-
Here , The dispersion number for a packed bed reactor using a pulse tracer is 0.140.
54
Page

CONCLUSION:-
The resistance time distribution function and concentration are initially increases with
time and then decreases. And according to this Variance will be change and dispersion
number will also change accordingly.
55
Page

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Chemical Reaction Engineering-I

CHEMICAL REACTION ENGINEERING-I

5th CHEMICAL (20CH502)

NAME :LATHIYA SARTHAK SURESHBHAI

Chemical Engineering Dept. GSFC University-Vadodara

Staff in-charge Course Coordinator

Chemical Engineering Dept. GSFC University-Vadodara

No. NAME OF EXPERIMENT DATE PAGE SIGN REMARKS

To determine the Order of reaction and activation

i) To plot RTD curve for a Packed Bed Reactor

Chemical Engineering Dept. GSFC University-Vadodara

EXPERIMENT NO-1 Date: _________

APPARATUS: - 1. Glass beaker

1. 0.1 N Na2S2O3 .5H2O

The reaction between sodium thio-sulphate and HCl is given by,

Na2S2O3 .5H2O + 2HCl → 2NaCl + 6H2O + SO2 + S

which precipitates sulfur.

The rate of reaction of sodium thiosulfate is given by,

Taking log on both side,

Chemical Engineering Dept. GSFC University-Vadodara

From this equation, activation energy also can be determined.

Chemical Engineering Dept. GSFC University-Vadodara

1. Prepare 250 ml of 0.1 N sodium thiosulfate and 250 ml of 1 M HCl solution.

Chemical Engineering Dept. GSFC University-Vadodara

No Volume Volume Concentr Volume of 1 Time Rate Log(r Log(Co

1 50 0 0.1 10 25.6 0.0039 -5.54 -2.3

2 40 10 0.08 10 31.7 0.00315 -5.76 -2.52

3 30 20 0.06 10 43.1 0.00232 -6.06 -2.81

4 20 30 0.04 10 70.85 0.00141 -6.56 -3.218

5 10 40 0.02 10 222 0.00045 -7.7 -3.91

No Volume of Volume Volume Concentrat Time Rate Log(r Log(Co

1 10 0 50 1 155 0.006 -5.025 0

2 10 10 40 0.8 158 0.006 -5.029 -0.22

3 10 20 30 0.6 152 0.006 -5.02 -0.51

4 10 30 20 0.4 170 0.0058 -5.14 -0.91

5 10 40 10 0.2 156 0.006 -5.026 -1.6

Chemical Engineering Dept. GSFC University-Vadodara

Sr Temperatur Concentration Volume Time taken Rate Rate

1 Slope of graph of log(rate) versus log(thiosulfate) = ____1_____

2 Slope of graph of log(rate) versus log(HCl) = _____0_____

3 Activation Energy E = _____56.025______J/mol

Rate = k CAn CBm

Where, A = Sodium thiosulfate

As volume of HCl is constant, m = 0

So, Rate = k CAn CBm = k’ CAn

Taking log on both side, we get,

Now, on plotting graph, we get,

log(Rate) versus log(Concentration of Sodium thiosulfate)

Chemical Engineering Dept. GSFC University-Vadodara

Rate = k CAn CBm

Where, A = Sodium thiosulfate

As volume of Sodium thiosulfate is constant, n = 0

So, Rate = k CAn CBm = k’ CBm

Taking log on both side, we get,

Now, on plotting graph, we get,

log(Rate) versus log(Concentration of HCl)

We know that, Arrhenius law is given as

Chemical Engineering Dept. GSFC University-Vadodara

(Rate)2 / (Rate)1 = (E/R) (1/T1 – 1/T2)

On putting values from table 3, we get,

1 Slope of graph of log(rate) versus log(thiosulfate) = 1_

2 Slope of graph of log(rate) versus log(HCl) = _0_

3 Activation Energy E = _56.025__J/mol

Reaction temperature : 31°C____

Reaction temperature : ___30 C_