Liquid Phase Chemical Reactor Final
Liquid Phase Chemical Reactor Final
Liquid Phase Chemical Reactor Final
0 Abstract
This experiment involves the saponification reaction of 0.1M Ethyl Acetate (EtOAc) with 0.1M
Sodium Hydroxide (NaOH). The purpose of this experiment is to gain familiarity with the
analytical procedure needed to establish the extent of this reaction from measurements of
concentration. A known volume of sample is run into an excess of 0.1M Hydrochloric Acid
solution (HCl) of known concentration for quenching of the solution. The remaining excess
hydrochloric acid is then determined by titration with standardised NaOH. Graphs of
x
a(ax)
against time were plotted to determine the gradient which represented the rate
constant, k2. Instead of gradually increasing from lower temperatures to higher temperature,
some values of k2were found to be increasing instead of decreasing and vice versa. Graphs of
concentration of reacted NaOH against time and
1
concentrationof reacted NaOH
against time
were plotted, whereby the order of the rate of reaction was found to be of second order
irrespective of changes in temperature.
1|Page
2.0 Introduction
In chemical engineering, the chemical reactor is the heart of the majority of chemical processes
since it is here that the raw materials react to form a required product. Thus, the design and
operation of chemical reactors are important aspects of the industrial operation.
However, reactors can take a wide variety of forms depending on the chemical process involved,
but the simplest for laboratory study is the homogeneous stirred-vessel type in which the
reactants are in liquid form under isothermal and adiabatic conditions. The reactor is basically
self-contained, and it may be operated batch-wise or as a continuous process. There is a gas inlet
to the reactor vessel for gas or liquid reaction. The vessel may be heated or cooled to allow either
exothermic or endothermic reactions to take place.
This experiment was conducted to study the analysis of reactants and products for a
saponification by titration that is, by determining whether the rate of reaction is a first or second
order reaction.
For the experiment conducted in the Chemical Engineering Lab, we used a 4000ml beaker as
reactor. Since both reactants were added at the same time, that is there were no outlets or inlets,
the reactor is considered to be a batch reactor in this case. Sampling was taken at 5minutes time
intervals.
2|Page
Figure 1 - CSTR
(Source:
https://upload.wikimedia.org/wikipedia/commons/thumb/b/be/Agitated_vessel.svg/2000pxAgitated_vessel.svg.png)
To study the analysis of reactants and products for a saponification reaction by titration.
To determine the effect of residence time onto the reaction extent of conversion.
3|Page
4|Page
Figure 2: The progress of a simple reaction showing the change in the number of A and B
molecules over a period of 1 min.
(Source: http://2012books.lardbucket.org/pdfs/principles-of-general-chemistry-v1.0/s18chemical-kinetics.pdf)
From the above graph, it is observed that the mixture initially contains only A molecules
(purple). With increasing time, the number of A molecules decreases and more B molecules
(green) are formed (top).
Rate of reaction is also defined to be proportional to the concentration of reacting species raised
to a certain power called the order of reaction. It is usually taken as the rate at which the reactant
disappear or the rate at which the product is formed.
The rate constant, K quantifies the speed of a chemical reaction. The reaction rate constant can
be determined graphically.
5|Page
Consider a chemical reaction where substance A and B are reacting to produce C, then, the
reaction rate has the form:
A+B
r = K [A]m [B]n
Where,
r: rate of reaction
K: rate constant (which depends on temperature)
m and n: Order of reaction
Rate constant is the rate of reaction when the concentration of each reaction is taken as unity. It
is a measure of the rate of reaction, therefore, the greater the value of the rate constant, the faster
the reaction. Each reaction has a definite value of the rate constant at a particular temperature
and the value of the rate constant for the same reaction changes with temperature. Moreover, the
6|Page
values of the rate constant do not depend upon the concentration of reaction but depend upon
order of reaction.
Figure 4: Expected shape for reactant concentration v/s time and (straight line plot to determine
rate constant) for a zeroth order reaction.
(Source: http://2012books.lardbucket.org/pdfs/principles-of-general-chemistry-v1.0/s18chemical-kinetics.pdf)
7|Page
Figure 5: Expected shape for reactant concentration v/s time and the natural logarithm of
reactant concentration v/s time (straight line plot to determine rate constant) for a first order
reaction.
(Source: http://2012books.lardbucket.org/pdfs/principles-of-general-chemistry-v1.0/s18chemical-kinetics.pdf)
8|Page
Figure 6: Expected shape for reactant concentration v/s time and the 1/reactant concentration
v/s time (straight line plot to determine rate constant) for a second order reaction.
(Source: http://2012books.lardbucket.org/pdfs/principles-of-general-chemistry-v1.0/s18chemical-kinetics.pdf)
The reaction chosen for this experiment is the saponification of ethyl acetate (EtOAc) with dilute
sodium hydroxide (NaOH).
NaOH + EtOAc
NaOAc + EtOH
4.0 Methodology
9|Page
C2H5CO2Na + CH3OH
(Figure 7 17/08/2016)
0.1 M Ethyl Acetate (EtOAc)
(Figure 8 -17/08/2016)
10 | P a g e
(Figure 9 17/08/2016)
Phenolphthalein Indicator
1000 cm3 volumetric flasks
2000 cm3 beakers
50 cm3 burette of accuracy 0.05 ml
Rubber Bulb Pipette filler
(Figure 10 : 17/08/2016)
3
25 cm pipette
Conical flasks
11 | P a g e
(Figure 11 : 17/08/2016)
Small beakers
Magnetic stirrer
Thermometers
Water bath
4.2 Procedure:
Procedures for preparing the solutions of:
Sodium Hydroxide
1. An electronic scale is used to weigh in a dry beaker 4.08g of 0.1M NaOH pellets
provided.
2. The weighed pellets are dissolved with distilled water.
3. This solution is poured in a 1000 cm3 volumetric flask and bring up to mark with more
distilled water. The contents is well shaken thoroughly.
4. The above steps are repeated to prepare for another 1000 cm3 volumetric flask.
Ethyl Acetate
1. The electronic scale is used to weigh in a dry beaker 8.86g of 0.1M EtOA.
12 | P a g e
2. The weighed EtOA is poured in a 1000 cm3 volumetric flask and bring up to the mark
using distilled water. The contents is well shaken thoroughly.
Hydrochloric Acid
1. The electronic scale is used to weigh in a dry beaker 10.13g of 0.1M HCl.
2. The weighed HCl is poured in a 1000 cm3 volumetric flask that has already been half
filled with distilled water. The contents is well shaken thoroughly.
-
At room temperature
2. The prepared solutions of NaOH and EtOA is preheated to the required temperature
before mixing.
3. Steps 5 to 11 from the procedures is repeated at room temperature.
-
5.0 Results
Part 1: Concentration Calculations
14 | P a g e
Reactants:
For NaOH:
Purity = 98%
For 1 dm3 = 0.1 M NaOH
Mr (NaOH) = 40 g/gmol
Therefore, for 1 dm3 =
0.1 40
0.98
= 4.08g NaOH
For EtOAc:
Purity = 99.5 %
For 1 dm3 = 0.1 M EtOAc
Mr (EtOAc) = 88.11 g/gmol
Therefore, for 1 dm3 =
0.1 88.11
= 8.86g EtOAc
0.995
Quenching:
For HCL:
Purity = 36%
For 1 dm3 = 0.1 M HCL
Mr (HCL) = 36.46 g/gmol
Therefore, for 1 dm3 =
15 | P a g e
0.136.46
= 10.13g HCL
0.36
Part 2: Titration
Temperature- 24C
Time/min
Volume
of Molarity
sample(ml)
solution
HCl
0
5
10
15
20
25
30
Table 1
25
25
25
25
25
25
25
Amount
of
0.1
0.1
0.1
0.1
0.1
0.1
0.1
HCl
not
used
of
neutralizing
sample,
= 25ml c
16 | P a g e
c
0
18.8
21.0
22.0
22.2
22.3
22.3
b
25
6.2
4.0
3.0
2.8
2.7
2.7
1000
1
25
1000
y
2.5
0.62
0.4
0.3
0.28
0.27
0.27
(a-x)
0.1
0.0248
0.016
0.012
0.0112
0.0108
0.0108
Time/min
(a-x)/M
x/M
1/(a-x)/M
0
5
10
15
20
25
30
Table 3
0.1
0.0248
0.016
0.012
0.0112
0.0108
0.0108
0
0.0752
0.084
0.088
0.0888
0.0892
0.0892
22.73
40.32
62.5
83.33
89.29
92.59
92.59
90
x
a(ax)
0
30.323
52.5
73.333
79.286
82.593
82.593
f(x) = 3.47x
80
70
60
50
/(( ))/M-1
40
30
20
10
0
0
10
15
20
25
Time/min
Graph 1
x
a(ax)
Gradient of line of best fit represents the negative of second order rate constant, -k2
Therefore from graph above,
k2 at 24C = 3.474
17 | P a g e
30
35
For 1st sample taken, at 0<t<5, volume of NaOH used for titration = 14.0ml
At volume 14.0 ml,
x
a(ax)
= 12.727
12.727
3.474
= 3.66min
0.05
0.05
0.04
0.04
(a-x)/M
0.03
0.03
0.02
0.02
0.01
0
10
15
20
25
Time/min
18 | P a g e
30
35
100
90
80
70
60
1/(a-x)/M
50
40
30
20
10
0
0
10
15
20
25
30
35
Time/min
Graph 3
1
(ax)/ M
against time/min
Temperature - 40C
Time/min
Volume
of Molarity
sample(ml)
solution
HCl
0
5
10
15
20
25
Table 4
25
25
25
25
25
25
Time/min
0
5
10
15
20
25
19 | P a g e
0.1
0.1
0.1
0.1
0.1
0.1
c
0
21.7
22.2
22.7
22.7
22.7
b
25
3.3
2.8
2.3
2.3
2.3
of
y
2.5
0.33
0.28
0.23
0.23
0.23
(a-x)
0.1
0.0132
0.0112
0.0092
0.0092
0.0092
Table 5
Time/min
(a-x)/M
x/M
1/(a-x)/M
0
5
10
15
20
25
Table 6
0.1
0.0132
0.0112
0.0092
0.0092
0.0092
0
0.0868
0.0888
0.0908
0.0908
0.0908
54.35
75.76
100
108.7
108.7
108.7
120
x
a(ax)
0
65.758
79.286
98.696
98.696
98.696
f(x) = 5.12x
100
80
/(( ))/M-1
60
40
20
0
0
10
15
20
Time/min
Graph 4
20 | P a g e
x
a(ax)
25
30
Gradient of line of best fit represents the negative of second order rate constant, -k2
Therefore from graph above,
k2 at 40C = 5.1225
For 1st sample taken, at 0<t<5, volume of NaOH used for titration = 20.4ml
At volume 20.4 ml,
x
a(ax)
= 18.348
18.348
5.1225
= 3.58min
0.02
0.02
0.02
0.02
0.02
(a-x)/M
0.01
0.01
0.01
0.01
0.01
0.01
0
10
15
20
25
Time/min
21 | P a g e
30
120
110
100
90
1/(a-x)/M
80
70
60
50
40
0
10
15
20
25
30
Time/min
Graph 6
1
(ax)/ M
against time/min
Temperature - 60C
Time/min
Volume
of Molarity
sample(ml)
solution
HCl
0
5
10
15
20
Table 7
25
25
25
25
25
Time/min
0
5
10
15
20
22 | P a g e
0.1
0.1
0.1
0.1
0.1
c
0
21.0
21.2
21.2
21.2
b
25
4.0
3.8
3.8
3.8
of
y
2.5
0.4
0.38
0.38
0.38
(a-x)
0.1
0.016
0.0152
0.0152
0.0152
Time/min
0
5
10
15
20
Table 8
(a-x)/M
0.1
0.016
0.0152
0.0152
0.0152
x
a(ax)
1/(a-x)/M
x/M
52.08
62.5
65.79
65.79
65.79
0
0.084
0.0848
0.0848
0.0848
0
52.5
55.789
55.789
55.789
Table 9
60
f(x) = 3.7x
50
40
/(( ))/M-1 30
20
10
0
0
10
15
20
Time/min
Graph 7
x
a(ax)
Gradient of line of best fit represents the negative of second order rate constant, -k2
Therefore from graph above,
k2 at 60C = 3.697
For 1st sample taken, at 0<t<5, volume of NaOH used for titration = 20.2ml
23 | P a g e
25
x
a(ax)
= 14.088
14.088
3.697
= 3.81min
0.02
0.02
0.02
0.02
0.02
(a-x)/M
0.02
0.02
0.02
0.02
0.02
0
10
15
20
Time/min
24 | P a g e
25
70
f(x) = 0.61x + 56.25
65
60
1/(a-x)/M
55
50
45
0
10
15
20
25
Time/min
Graph 9
1
(ax)/ M
against time/min
Temperature - 20C
Time/min
Volume
of Molarity
sample(ml)
solution
HCl
0
5
10
15
20
25
30
35
40
Table 10
25
25
25
25
25
25
25
25
25
Time/min
0
5
25 | P a g e
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
c
0
18.0
b
25
7.0
of
y
2.5
0.7
(a-x)
0.1
0.028
10
15
20
25
30
35
40
Table 11
19.6
19.9
21.2
21.4
22.0
22.2
22.2
5.4
5.1
3.8
3.6
3.0
2.8
2.8
0.54
0.51
0.38
0.36
0.3
0.28
0.28
Time/min
(a-x)/M
x/M
1/(a-x)/M
0
5
10
15
20
25
30
35
40
Table 12
0.1
0.028
0.0216
0.0205
0.0152
0.0144
0.012
0.0112
0.0112
0
0.072
0.0784
0.0795
0.0848
0.0856
0.088
0.0888
0.0888
24.51
35.71
46.3
58.8
65.69
76.92
83.33
89.29
89.29
90
0.0216
0.0205
0.0152
0.0144
0.012
0.0112
0.0112
x
a(ax)
0
25.714
36.296
38.780
55.789
59.444
73.333
79.286
79.286
f(x) = 2.32x
80
70
60
50
/(( ))/M-1 40
30
20
10
0
0
10
15
20
25
Time/min
26 | P a g e
30
35
40
45
Graph 10
x
a(ax)
Gradient of line of best fit represents the negative of second order rate constant, -k2
Therefore from graph above,
k2 at 20C = 2.318
For 1st sample taken, at 0<t<5, volume of NaOH used for titration = 14.8ml
At volume 14.8 ml,
x
a(ax)
= 8.5098
8.5098
2.318
= 3.67min
0.05
0.04
0.04
0.03
(a-x)/M
0.03
0.02
0.02
0.01
0
10
15
20
25
30
35
Time/min
40
45
100
f(x) = 1.71x + 29.18
90
80
70
60
1/(a-x)/M
50
40
30
20
10
0
0
10
15
20
25
30
35
40
45
Time/min
Graph 12
1
(ax)/ M
against time/min
Temperature - 15C
Time/min
Volume
of Molarity
sample(ml)
solution
HCl
0
5
10
15
20
25
30
35
40
45
Table 13
25
25
25
25
25
25
25
25
25
Time/min
28 | P a g e
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
0.1
of
(a-x)
0
5
10
15
20
25
30
35
40
45
Table 14
0
19.3
21.4
22.2
23.0
23.6
23.8
23.9
24.2
24.2
25
5.7
3.6
2.8
2.0
1.4
1.2
1.1
0.8
0.8
2.5
0.57
0.36
0.28
0.2
0.14
0.12
0.11
0.08
0.08
Time/min
(a-x)/M
x/M
1/(a-x)/M
0
5
10
15
20
25
30
35
40
45
Table 15
0.1
0.0228
0.0144
0.112
0.008
0.0056
0.0048
0.0044
0.0032
0.0032
0
0.0772
0.0856
0.0888
0.092
0.0944
0.0952
0.0956
0.0968
0.0968
27.78
43.86
69.44
100
125
178.57
208.33
250
312.5
312.5
29 | P a g e
0.1
0.0228
0.0144
0.112
0.008
0.0056
0.0048
0.0044
0.0032
0.0032
x
a(ax)
0
33.86
59.444
79.286
115
168.571
198.333
217.273
302.5
302.5
350
300
f(x) = 6.7x
250
200
/(( ))/M-1
150
100
50
0
0
10
15
20
25
30
35
40
Time/min
Graph 13
x
a(ax)
Gradient of line of best fit represents the negative of second order rate constant, -k2
Therefore from graph above,
k2 at 15C = 6.6996
For 1st sample taken, at 0<t<5, volume of NaOH used for titration = 16.0ml
At volume 16.0 ml,
x
a(ax)
= 17.778
30 | P a g e
17.778
6.6996
= 2.65min
45
50
0.04
0.03
0.03
0.02
(a-x)/M
0.02
0.01
0.01
0
0
10
15
20
25
30
35
40
Time/min
31 | P a g e
45
50
350
300 f(x) = 6.94x + 6.68
250
200
1/(a-x)/M
150
100
50
0
0
10
15
20
25
30
35
40
45
50
Time/min
Graph 15
1
(ax)/ M
against time/min
6.0 Discussion
In this practical of saponification, the titration method was used with the purpose of finding the
reaction rate constant, k and the order of the reaction performed at the different temperatures
mentioned. Order of a reaction describes the mathematical form in which the results of the
changes during a chemical reaction can be demonstrated, while the reaction rate constant, k is the
constant of proportionality which relates the rate of a chemical reaction and the concentrations of
the reactants. (Laidler K J, 2015).
Order of reaction
From the shape of the graphs of a-x (M) v/s time (min) obtained, which represents the change of
concentration of reacted NaOH in the reactor with time, it can be deduced that the saponification
reaction between NaOH and Ethyl Acetate undergoes a 2nd order reaction. Graphs of
1
(ax)/ M
32 | P a g e
against time/min were also plotted to determine the order of reaction. Since the
line of best fit starts above the origin at t=0 for all experiments with different temperatures, it is
deduced that the reaction is of 2nd order. Moreover, the order of reaction is known to be
independent of temperature as orders change only when the reaction changes. (University of
Rhode Island, n.d). As it can be seen from our experiment, at all corresponding temperatures, the
order of reaction remained the same, i.e. of second order.
Rate constant
Furthermore, according to the Arrhenius equation, it is understood that as temperature increases
the reaction rate constant also increases. However, in the practical done, it is noted that there are
certain anomalies in the rate constants for the respective temperatures depicted on the graph. As
illustrated, at temperature 15 oC and 20oC, the rate constant decreases from 6.69 - 2.31 M -1/min,
and as from 20 40oc, it increases from 2.31 5.12 M -1 /min. This is supported by the fact that
not all points lie on the line of best fit for all graphs, for example at 24 oC,40 oC and 60oc, the
values of R2 are less than 0.75, which is not suitable. Eventually, the above mentioned
inaccuracies and discrepancies can be due to:
Contamination of equipment.
Ineffective stirring by magnetic stirrer.
Parallax error white reading the burette.
Error of apparatus.
Drop or rise in temperature of the batch reactor as the reaction was being carried out.
Human time error during sampling at different time intervals.
33 | P a g e
Type of Reactor
Batch Reactor
Area of Application
Batch processes are used in chemical (inks, dyes,
polymers) and food industry.
Reactor
reactions.
34 | P a g e
Figure 7 Checking condition inside the case of a continuous stirred tank reactor (CSTR).
(Source from: https://en.wikipedia.org/wiki/Chemical_reactor)
7.0 Conclusion
The purpose of this experiment is to carry out saponification reaction between NaOH and EtOAc
in a CSTR which also required to determine the effect of residence time onto the reaction extent
of conversion and to determine the reaction rate constant. Continuous stirred tank reactor is used
in this experiment in order to achieve the purpose of this experiment. After completing the
experiment, we are able to collect the data and all the purposes are achieved. (M.T. Jaafar, 2014)
According to the rate law and the corresponding rate constant K of any chemical reaction as the
temperature at each set of the experiment is increased, the corresponding K should increase.
As mentioned above from the discussion, the results of K did not support the relationship as
expected due to some inaccuracies.
35 | P a g e
The Arrhenius equation could be used to show the effect of a change of temperature on the rate
constant - and therefore on the rate of the reaction. If the rate constant doubles, for example, so
also will the rate of the reaction. (J. Clark, 2002)
There are a few recommendations that can improve the experiment result. With
recommendations such as wider range of temperature and variation of concentrations, the results
would be much better than before. This experiment is considered successful as all the purposes
are achieved.
8.0 References
StudeerSnel.nl. 2016. Practical - Lab report for reaction engineering - 302263: Reaction
Engineering 325 - StudeerSnel. [ONLINE] Available at:
https://www.studeersnel.nl/nl/document/curtin-university-of-technology/reactionengineering-325/practicum/practical-lab-report-for-reaction-engineering/625506/view.
[Accessed 09 October 2016].
36 | P a g e
Nurul Ain, Pegawai Kadet at Palapes Laut UMP. 2013. Chemical reaction engineering.
[ONLINE] Available at:
http://www.slideshare.net/NurulAin45/chemical-reaction-engineering-28330576.
[Accessed 9 October 2016].
Clark J., 2013. Rate constants and the arrhenius equation [Online] Available from:
http://www.chemguide.co.uk/physical/basicrates/arrhenius.html [Accessed 08 Oct. 2016]
37 | P a g e
Rate constants and the arrhenius equation. 2002. [ONLINE] Available at:
http://www.chemguide.co.uk/physical/basicrates/arrhenius.html. [Accessed 12 October
2016].
38 | P a g e