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Title of Experiment
(Experiment No. 8) (Sequence No. 3)
Date of Experiment:
(Regular/Make-up)
Regular
(Regular/Make-up)
Regular
Group No.:
Batch:
1. Smriti Agrawal
2. Mounica Bodapudi
3. Lavanya
4. Nidhi Rajwania
Name of TA:
19/01/2012
-
6
Thursday
Y9587
Y9175
Y9368
Y9306
Shilpi Saxena
Marks: ______________
I/C
Prof. P. K. Bhattacharya
Dr. Sri Sivakumar
Content
1.
2.
3.
4.
5.
6.
7.
8.
9.
Introduction
Objective
Theory
Keywords
Procedure
Observation
Calculation
Discussion
Error analysis
Page no.
3
3
3
3
6
7
8
11
11
OBJECTIVE
To determine the reaction rate of the saponification reaction
at ambient conditions and determine the reaction rate
constant for it
To verify the order of the reaction
Keywords
CSTR, reaction rate constant, order of reaction
Relevant Reaction
NaOH + CH3COOC2H5
CH3COONa + C2H5OH
C+D
With CAO = CBO and under constant volume condition rate (for a
second order reaction) can be
represented as
-rA = -dCA/dt = KCA2
=VR/VO = CAO*XA/ (-rA) = (CAO- CA)/ (-rA) =(CAO- CA)/ KCA2
(1)
Degree of conversion,
XA = (CAO- CA)/CAO
(2)
and
rate of reaction,
-rA = CAO*XA/ , g mol/ L min
(3)
the rate constant,
K = (CAO- CA)/ CA2, L/g mol min
(4)
For nth order reaction,
-rA =K CAn
log(-rA) = log K + n*logCA
The order of the reaction, n, can be obtained from a plot of log (rA) vs. log CA, that yields a straight line with slope = n, and
intercept (at CA = 1 or at log CA = 0) shall give the value of log(K).
Also, a plot of vs. XA/(1-XA)2 shall yield a straight line for an
assumed second order reaction with slope = 1/(KC AO). From this
slope, rate constant K can be obtained. [2]
APPARATUS REQUIRED
1) Electricity supply: single phase, 220 VAC, 50 Hz, 5-15 Amp
socket with earth connection
2) Distilled water (to prepare solution)
3) Drain required
4) 5 conical flasks
5) Measuring cylinder
6) 2 stopwatches
7) Burette
8)
Chemicals:
NaOH pellets
N/10 HCl
Ethyl acetate
Indicator(phenolphthalein)
Quantity:
100 g
100 ml
200 ml
few drops
EXPERIMENTAL PROCEDURE
1) Firstly, the reactant solutions to be used for the experiment
were prepared.
20 L of 0.1N NaOH solution by dissolving 80gm NaOH in 20L
water and
20 L of 0.1N CH3COOC2H5 solution by mixing 200.24 ml
CH3COOC2H5 in 20L water.
2) The respective tanks were filled with these solutions and the
motor was switched on to fill them into their respective overhead
tanks.
3) Equal volumetric flow rates of both NaOH and CH 3COOC2H5
were fed into the CSTR. The flow rates of the streams were
measured with the Rotameter.
4) When the liquid in the reactor reached a certain level (nearly
3/4th) it started overflowing and the volume of liquid inside it
became constant. It was at this instance that the stirrer of the
CSTR was switched on.
5) Next, the heater, provided on the set-up, was switched on and
a desired temperature was set on its digital controller.
6) An experimental measurement of the flow rate was made by
collecting the product stream in a measuring cylinder for a certain
time period, measured on a stopwatch. This flow rate was used to
make an estimate of the residence time for the reactor.
7) Once the desired temperature was reached, it was assured
that the reactor had reached steady state by allowing it to run
undisturbed for 10 minutes or the calculated residence time,
whichever was greater.
8) A 10ml sample of the product was taken from the outlet of the
CSTR and was added to20ml 0.1N HCl kept in a flask.
9) The solution left in the flask was titrated with 0.1N NaOH
which was added drop by drop from a burette, using
phenolphthalein as indicator. The volume of NaOH (V NaOH) required
for the complete neutralization of the leftover HCl was noted.
10) The steps 3 to 9 were repeated for different values of
temperatures and different flow rates for each value of
temperature.
11)The experiment was conducted at 40,50 and 600oC and the
flow rates used for each temperature were 7.5,12.5 and 15 LPH,
as measured by the Rotameter.
Observations:
T=16 oC
Rotamet
er
reading
Volume
in ml
t,Reside
nce time
in min
Initia Final
l
NaO
NaOH H
Differe
nce
57
Time in Flow
s
rate
in
l/min
14.44
0.24
7.5
9.08
10.0
37
6.10
0.36
5.9
12.5
44
5.72
0.461
5
5.41
41
58
63
55.4
3.0
20.0
37.0
55.0
72.5
1.0
18.0
58
75.2
80
72.4
19.5
36.5
55.0
72.5
89.5
18.0
35.3
17
17.2
17
17
16.5
16.5
18.0
17.5
17.0
17.0
17.3
Volume
in ml
Time in Flow
s
rate
Initia
l
Final
NaO
Differe
nce
T=28 oC
Rotamet
er
t,
Residen
reading
7.5
35
7.40
in
l/min
0.28
ce time
in min
7.58
NaOH H
10.0
47
7.00
0.40
5.33
12.5
51
6.37
0.48
4.47
Rotamet
er
reading
Volume
in ml
t,Reside
nce time
in min
Initia Final
l
NaO
NaOH H
Differe
nce
7.5
79
Time in Flow
s
rate
in
l/min
18.87
0.25
8.56
10.0
48
7.56
0.38
5.64
12.5
39
5.56
0.42
5.12
52.0
20.0
38.2
58.0
22.0
55.8
74.6
30.0
14.0
32.0
51.0
69.0
18.6
18.2
18.6
18.8
18.8
18.8
19.0
19.0
18.0
19.0
18.0
18.4
35.3
53.2
2.0
19.8
37.8
55.8
3.0
21.2
39.4
57.2
16.2
34.0
53.2
71.0
19.8
37.8
55.8
74.2
21.2
39.4
57.2
75.0
34.0
52.0
17.9
17.8
17.8
18.0
18.0
18.4
18.2
18.2
17.8
17.8
17.8
18.0
T=38 oC
70.6
38.2
56.8
76.8
38.8
74.6
93.6
49.0
32.0
51.0
69.0
87.4
SAMPLE CALCULATION
T= 150C
Flow rate = 7.5 LPH
In this manner,
and
CASE 1
T= 150C
NaO
H
(LPH
)
7.5
10.0
12.5
ETOAc (mi
(LPH)
n)
9.07
7.5 8
5.90
10.0
0
5.41
12.5
0
Buerette
Reading
(ml)
17.0
NaOH
consumed
(mMol)
1.73
CAO (M)
CA (M)
XA
0.050
0.028
0.43
1.32
16.5
1.68
0.050
0.033
0.33
0.73
17.0
1.73
0.050
0.028
0.43
1.32
`Residence Time vs
Slope= 1/K
= 2.197
K= 9.103
CASE 2
T= 28 0C
NaO
H
(LPH
)
7.5
10.0
12.5
ETOAc
(LPH)
7.5
10.0
12.5
(mi
n)
7.5
8
5.3
3
4.4
7
Buerette
Reading
(ml)
NaOH
consumed
(mMol)
18.4
1.81
CAO (M)
CA (M)
XA
0.050
0.014
0.71
8.79
18.2
1.86
0.050
0.016
0.67
6.35
17.8
1.83
0.050
0.020
0.59
3.58
Residence Time vs
10
CASE 3
T= 360C
NaO
H
(LPH
)
7.5
10.0
12.5
ETOAc
(LPH)
7.5
10.0
12.5
(mi
n)
8.5
6
5.6
4
5.1
2
Buerette
Reading
(ml)
18.8
NaOH
consumed
(mMol)
1.89
CAO (M)
CA (M)
XA
0.050
0.012
0.75
18.8
1.91
0.050
0.010
0.80
18.0
1.91
0.050
0.010
0.80
Residence Time vs
11
12.64
19.16
19.16
K= 11.567
T
288
299
309
-1/T
-0.00347
-0.00334
-0.00324
K
9.103
10.219
11.567
Ln(K)
2.2308
2.3242
2.4481
12
RESULT
(A)
Temperature
Value of K
(Kelvin)
288
299
309
9.103
10.219
11.567
Logarithmic form:
Error analysis
1. Slope of the first graph comes out to be ve . This can be
due to the following errors:
Time lag in which solution was taken and the
titration was conducted. So, the reaction
continued and concentrations changed.
Titration was erroneous. The pink solution stability
and first appearance, or presence of some water
in the flask.
Dropper used may be of other chemical.
13
14