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UNIVERSITI TEKNOLOGI MARA

FACULTY OF CHEMICAL ENGINEERING


PROCESS ENGINEERING LABORATORY II
(CPE 554)

NAME

: AMIR FADZRUL BIN AB RAHMAN (2012289094)


: HAFIFAH AMIRAH BT AKHAWAN (2012416828)
: AHMAD HILMI BIN ISMAIL
(2012622876)
: HAMZAH BIN ANUARULHADI
(2012898932)
GROUP
: EH2214C
EXPERIMENT
: SHELL AND TUBE HEAT EXCHANGER
DATE PERFORMED
: 2 APRIL 2013
SEMESTER
: MARCH- JULY 2013
PROGRAMME/ CODE : EH221
SUBMIT TO
: SITI SHAWALLIAH IDRIS

No.
1.

Title
Abstract/summary

Allocated marks (100%)


5

2.

Introduction

3.

Objectives/aims

4.

Theory

5.

Materials and apparatus

6.

Methodology/procedure

10

7.

Result

10

8.

Calculation

10

9.

Discussion

20

10. Conclusion

10

11. Recommendation

12. References

Marks

13. Appendix

5
Title
TOTAL MARKS

100

Page Number

Abstract
Introduction
Objectives
Theory
Apparatus
Methodology/Experimental Procedures
Results
Calculations
Discussions
Conclusion
Recommendations
Appendices
Remarks:
Checked by:

Rechecked by:

..

Date:

CONTENT

ABSTRACT
Reactor is a device or process vessel that used in industrial plant in which chemical reaction take
place. In this experiment, the temperature of the reactor needs to be varied which is 40 oC, 50oC
and 60oC in order to study the effect of temperature and reaction time and to determine the
relationship between reaction rate with conversion, reactor volume and feed rate. 50 mL of
samples were collected in conical flask that contained 3 drops of phenolphthalein and 10 mL of
0.25M HCl in every 1, 5, 10, 15, 20 and 25 minutes for each temperature. The samples then
titrated with 0.1M of NaOH until pale pink colour formed. From the data obtained, the
conversion of NaOH was calculated and the result was plotted in the graph. Temperature 40 oC
shows a little increment from 84.80% in minute 1 to 87.20% in minute 25. For temperature 50 oC
and 60oC, the conversion shows a decreasing pattern from minute 1 to minute 25 which are
90.40% to 80.80% and 84.80% to 79.20% respectively. However, the effect of temperature and

reaction time cannot be determined as the k values obtained from the graph plotted were negative
except for temperature 40oC. When the k values negative, activation energy, Ea cannot be
evaluated as it will approach math error. In conclusion, the conversion of NaOH for each
temperature were successfully determined but for overall, the experiment can be considered as
failed because the effect of temperature and reaction time cannot be study as the value of k is
negative in temperature 50oC and 60oC due to the some error made.

INTRODUCTION
OBJECTIVES

To determine the effect temperature on reaction rate constant, k for batch reaction and to
determine the activation energy of saponification.

THEORY
APPARATUS

Continuous stirred tank reactor ( Model BP:100), stopwatch, beakers, pipet, measuring cylinder,
0.1M NaOH, 0.1M ethyl acetate, 0.25M HCl.

Figure 1: Continuous stirred tank reactor (Model BP:100)

PROCEDURE

1. The pump P1 was switched on to start on pumping 1.25 liters of 0.05M ethyl acetate form
the feed tank into reactor. The pump P1 stopped.
2. Then the pump P2 was switched on and started to pump another 1.25 liters of the0.05M
NaOH into the reactor. The pump P2 was being stopped when the 2.5 liters of volume are
reached. The stirrer and heater were switched on and the temperature was set to be 40C.
The time was recorded.
3. 10ml of the 0.25M HCL with 3 drops of phenolphthalein was prepared in the beakers.
4. After 1 minute of reaction, sampling valve V7 was opened to collect 50ml sample. 10 ml
of the sample was added to the 0.25M HCl immediately.
5. The mixture was titrated with the 0.1M NaOH.
6. Steps 4 and 5 were repeated for reaction times of 5, 10, 15, 20 and 25
7. The experiment was repeated for reaction temperatures 50C and 60C.

RESULT

Table 1: Effect of Retention time to conversion (X), rate constant (k) and rate of reaction (Retention
time (min)

Volume of
Conversion, X
NaOH
(%)
titrated (mL)
1
21.2
84.80
5
21.4
85.60
10
21.4
85.60
15
21.6
86.40
20
21.6
86.40
25
21.8
87.20
rA) at room temperature (40 C)

Retention
time (min)
1
5
10
15
20
25

Volume of
NaOH
titrated (mL)
22.6
22.2
21.8
21.7
20.0
20.2

Conversion, X
(%)
90.40
88.80
87.20
86.80
80.00
80.80

Rate constant, k
(Lmol-1min-1)

0.0064

Rate constant, k
(Lmol-1min-1)

-0.038

Rate of reaction,
-rA

0.0064 Ca2

Rate of reaction,
-rA

-0.038 Ca2

Table 2: Effect of Retention time to conversion (X), rate constant (k) and rate of reaction (rA) at room temperature (50 C)

Table 3: Effect of Retention time to conversion (X), rate constant (k) and rate of reaction (Retention
time (min)

Volume of
Conversion, X
NaOH
(%)
titrated (mL)
1
21.2
84.80
5
20.1
80.40
10
19.7
78.80
15
20.8
83.20
20
19.8
79.2
25
19.8
79.2
rA) at room temperature (60 C)

Rate constant, k
(Lmol-1min-1)

-0.0086

Rate of reaction,
-rA

-0.0086 Ca2

Conversion VS Space time


100
80
40C

60

Conve rsion, X

50C

40

60C

20
0
0

10

15

20

Space time , (min)

25

30

ln (Cao/Ca) VS Space time


5
4

40C
Linear (40C)

ln (Cao/Ca)

50C

Linear (50C)

f(x) = - 0.03x + 2.37


f(x)
0.01x + 1.89
R ==
f(x)
=0.91
- 0.01x + 1.77
R = 0.93
R = 0.33

60C
Linear (60C)

0
0

10

15

20

25

30

Space time , (min)

CALCULATIONS

Calculation of the Conversion in reactor, X from back-titration method


Volume of sample
Concentration of NAOH in feed vessel

= Vs
= Ca,f

=
=

50 mL
0.1 M

Volume of HCl for quenching


Concentration of HCl in standard solution
Volume of titrated NaOH
Concentration of NaOH used for titration

= VHCl,s

Conc. Of NaOH entering reactor, Cao

=
= CHCl,s =
= V1
= Ca,s
C a,f
=
2

10 mL
0.25 M
=
21.2 mL
=
0.1 M

Ca, s
V 1
C HCl , s

0.05 M

8.48 mL

Volume of unreacted quenching HCl, V2

Vol. of HCl reacted with NaOH in sample, V3

1.52 mL

Moles of HCl reacted with NaOH in sample, n1

= VHCl,s - V2
C HCl, s V
=
1000

0.00038 mol

Moles of unreacted NaOH in sample, n2

= n1

0.00038 mol

Conc. Of unreacted NaOH in the reactor, Ca

0.0076

Conversion of NaOH in the reactor, X

n2
Vs
1000

( )

Ca
C a0

x100% =

84.80%

Determination of rate constant, k


A graph of 1/Ca vs t was plotted and the equation of the straight line obtained was:
y= 0.0064x + 1.8869

(Equation 7.1)

Comparing with the equation below:


ln (Cao/Ca) = kt + 1/Cao

(Equation 7.2)

Hence the value of k was found to be 0.0064 Lmol-1min-1.

DISCUSSIONS
The objectives of this experiment were to determine the reaction rate and the relationship
between conversions, reactor volume and feed rate. The other aim that needs to be study was the

relation between temperature and reaction rate. In this experiment, the reaction between sodium
hydroxide, NaOH and ethyl acetate, Et(Ac) was conducted in a batch mode.
The conversion of each retention time at room temperature was calculated and graph of
conversion versus space time was plotted. Based on the result obtained for temperature 40 oC,
there was a little increasing of NaOH conversion from minute 1 to minute 25 which is from
84.80% to 87.20%. It shows that as the space time increase, the conversions of NaOH also
increase. This relation formed due to the theory stated that when the time is longer, more
reactants can react to each other and form products until the maximum conversion achieved.
However, the trend of plotted graph for the temperature 50 oC and 60oC were different
compare to the 40oC which is keep decreasing as the time passed by until minute 25. For
temperature 50oC, the conversion of NaOH decreased from 90.40% in minute 1 to 80.80% in
minute 25. While, for temperature 60oC, the conversion show some fluctuated trend as in minute
1 to minute 10 it decreased from 84.80% to 78.8%. In minute 10 to minute 15, the conversion
changed from 78.8% to 83.20%. It shows some increment but in minute 15 to minute 20, the
conversion of NaOH decreased again to 79.2%. In minute 20 to minute 25, the conversion
remained constant at 79.2%. The decreasing of conversion at temperature 50 oC and 60oC were
because of the reaction between NaOH and Et(Ac) was too slow and only converted small
amount of reactant into products. Both data obtained for temperature 50 oC and 60oC did not
complied with the theory as there were some error were made.
For effect of temperature and reaction time, the constant k for each temperature needs to
be determined by plotting the graph of ln (Ca0/Ca) versus space time. In the end of the
experiment, the constant k obtained for temperature 40oC was 0.0064 Lmol-1 min-1. While for
temperature 50oC and 60oC were -0.0308 and -0.0086 Lmol-1 min-1. As the k values of 50oC and
60oC were in negative, the effect of temperature and space time cannot be determined as it will
reach math error. Therefore, the activation energy, Ea also cannot be evaluated and this
experiment was considered to be failed due to some error made. The flask did not washed cleanly
after using for other reaction of chemical. Thus, it can cause error during titration with NaOH
and form dark purple colour even the sample have been titrated slowly. It can be concluded that
the conversion of NaOH for each temperature were successfully obtained but totally failed for
overall experiment as the effect of temperature and reaction time cannot be determined.

CONCLUSIONS
In the end of this experiment, the aims of the experiment were not successfully achieved. Only
for the conversion of NaOH can be determined. Besides, only temperature of 40 oC complied
with the theory which is as the space time increases, the conversions of NaOH also increase. It
proves that when the time is longer, more reactants can react to each other and form products
until the maximum conversion achieved. For temperature 50 oC and 60oC, the conversions of
NaOH were decreased from minute 1 to minute 25. So it is not complied with the theory stated.
For overall experiment, it can be considered as failed because the effect of temperature and
reaction cannot be determined. This is because, the k values obtained were in negative value.
Thus, it will reach math error and the activation energy, Ea also cannot be evaluated.

RECOMMENDATIONS
1. The apparatus should be clean thoroughly to avoid contamination.
2. Titration should be done carefully so that accurate reading could be obtain.
3. The readings should be taken at least 4 different temperatures so that we can obtain
a better graph to find the activation energy.