Chemical Reactor Experiment

CHE132L – Chemical Engineering Laboratory 2 / T

4th term of A.Y. 2017-2018

ABSTRACT To further demonstrate the topics stated

above, the kinetic study of one of the most well-known
The objective of the study was to
reactions in chemistry will be performed. This reaction
demonstrate the saponification reaction of ethyl
is the saponification of ethyl acetate and sodium
acetate and sodium hydroxide. Same initial
hydroxide. It is an overall second order and first order
concentration of 0.1 M was used in the experiment.
with respect to each reactant. In the reaction,
Conductimetric data was used to calculate the
hydroxyl ions are consumed and acetate ions are
reaction conversion of 84.82%. Using various
produced (Ullah, Ahmad, & Younas, 2015).
chemical kinetics principles and design equation, the
Conductimetric measurement will be used to
rate constant, 0.03516 L-mol-1s-1 and rate of reaction,
determine the composition at any time. Since
𝑚𝑜𝑙
8.1047 𝑥 10−6 , were obtained. Graphical hydroxyl ions are more conductive than acetate ions,
𝐿−𝑠

representations were also used in order to show that a decrease in the conductivity will be observed.
the reaction is in fact a second order reaction. the
Batch reaction will be performed in order to
experimental results are believed to be within the
get the conductivity vs. time data, rate of reaction, rate
reasonable values based on previous studies of the
constant, and conversion over time using the design
same saponification reaction.
equation below.

𝑑𝐶𝑎
INTRODUCTION = −𝑘𝐶𝑎2
𝑑𝑡
Chemical kinetics and reactor design are the 𝐶𝑎
𝑑𝐶𝑎 𝑡
∫ 2
= −𝑘 ∫ 𝑑𝑡
key factors for producing almost all industrial 𝐶𝑎𝑜 𝐶𝑎 0

chemicals. It known that the knowledge of chemical

1 1
kinetics and reactor design makes chemical − = 𝑘𝑡
𝐶𝑎 𝐶𝑎𝑜
engineers distinguishable among other engineers.
1 1 1
The chemical kinetic principles applied in chemical 𝑡= ( )−
𝑘𝐶𝑎𝑜 1 − 𝑥𝑎 𝑘𝐶𝑎𝑜
plants can also be used in other areas such as, waste
treatment, air and water pollution. The objective of the
Equation 1. Second-order batch reaction design
equation
experiment is to demonstrate chemical reaction
engineering topics. Its main concern are the
mechanisms of the reaction and other factors that
control the reaction process (Fogler, 2004).

Experiment 1. Chemical Reactor Experiment

CHE132L - T BS in Chemical Engineering
EXPERIMENT OBJECTIVES
1. To calibrate the peristaltic pumps of the
reagents to obtain the reagents flow
measurements.
2. To determine the ionic conductivities that
are necessary for the treatment of
experimental data in the next exercises.
3. To demonstrate the saponification of
ethyl acetate with sodium hydroxide and
the obtention of the reaction order.
METHODOLOGY
Materials
1. QRCA/QRCAC Edibon Unit
2. 0.1 M Sodium Hydroxide Solution
3. 0.1 M Ethyl Acetate Solution
4. Conductivity Meter
Determination of ionic conductivities, reaction order,
reaction constant, and specific rate of reaction
1. Switch ON the unit and the software
2. Place 500 mL of 0.1M NaOH inside the
reactor.
3. Add 500 mL of 0.1M Ethyl Acetate and
immediately turn on the stirrer and set it to
100% agitation rate.
4. Place the conductivity meter after the last
drop of ethyl acetate and record the initial
conductivity.
5. Record the conductivity until it becomes
stable.
6. Determine the order of reaction. reaction
constant, and specific rate of reaction.

DATA AND RESULTS

Procedure
The saponification of ethyl acetate and
Calibration of Peristaltic Pumps
sodium hydroxide was performed and kinetic data
1. Before the calibration process, the
was obtained by the measurement of conductivity
pumps must be manually primed.
over time. Figure 1 shows the conductivity vs. time
2. To prime the pumps, fill the reactor with
graph.
250 mL water. Open the valves and let
the water flow back into the tubes. 10
3. Once the air bubbles are completely Conductivity vs. Time
removed, close the valves to stop the 8

water from flowing back into the reagent 6

Conductivity, mS

bottles and start the calibration process.

4
4. Fill up the two reagent bottles with 1L of
water each 2
5. Fill the tank with 500 mL water Time, s
0
6. Activate AB-2 pump and set it to 100%
0 1000 2000 3000 4000 5000 6000
7. Simultaneously record the time to fill up
Figure 1. Conductivity vs. Time graph
every 20 mL volume (20 mL, 40 mL, 60
mL, 80 mL and 100 mL)
In order to interpret the conductivity data into
8. Repeat the process for the other pump
conversion, an equation was calculated by linear
AB-3.
regression using the data shown in Table 1. The
2
assumptions for the equation is that at the start of the order reaction. To prove that the experiment
reaction, the conversion is 0% and when the performed demonstrated a second order reaction,
conductivity becomes stable, the reaction conversion Equation 1 was used and the calculated values where
is 100%. graph and is shown in Figure 3. The r2 = 0.9689.

2nd Order Reaction t > 1500 s

Table 1. Data for conversion equation.
80
Time, s Conductivity, Conversion R² = 0.9689
60
mS %

1/1-x
40
0 9.37 0 20
5420 3.7 100 0
0 2000 4000 6000
Time , s
By linear regression, the equation to interpret
the conductivity to reaction conversion was obtained
Figure 3. Second-order reaction graph
and is shown in equation 2.

Figure 2 shows that the reaction is in second

𝑦 = 1.6253 − 0.1764 𝑥
order but at t > 2000s, discrepancies from the
Equation 2. Conductivity to reaction conversion
trendline can be observed. It is due to presence of the
equation
product as the reaction proceeds. By observing the
where,
reaction at t < 1500s, the graph shown in Figure 4,
y - conversion
shows that at earlier stages of the reaction, it
x - conductivity
demonstrates a second order reaction.

Using equation 2, the conversion data over 2nd order reaction t < 1500 s
time was obtained and is shown in Figure 2. 8
6 R² = 0.9964
1/1-x

4
Conversion vs. Time 2
1 0
0.8 0 500 1000 1500 2000
Conversion

0.6 Time, s
0.4
0.2
Figure 4. Second order reaction graph at t<1500s
0
20 920 1820 2720 3620 4520 5420
Time, s With this, the data for calculation of rate
constant and rate of reaction will be at t < 1500s. The
Figure 2. Conversion vs. Time graph
overall reaction conversion is 84.82%. Using
Equation 1, the calculated average rate constant is
Based on past kinetic study of the
0.03516 L-mol-1s-1. The rate of reaction will be
saponification reaction of ethyl acetate and sodium
calculated using Equation 3. The rate of reaction is
hydroxide, the reaction is said to be an overall second 𝑚𝑜𝑙
8.1047 𝑥 10−6 .
𝐿−𝑠
3
 2 (1
−𝑟𝑎 = 𝑘𝐶𝑎𝑜 − 𝑥)2
Equation 3. Rate of reaction equation

ANALYSIS, INTERPRETATION, & CONCLUSION

During the experiment, the saponification of

ethyl acetate and sodium hydroxide was examined.
The reaction progression was tracked by real-time
conductivity measurement.
It was observed that as the reaction
proceeded, there was a decrease in the conductivity
values. A reaction conversion of 84.82%, rate
constant of 0.03516 L-mol-1s-1, and the rate of
𝑚𝑜𝑙
reaction of 8.1047 𝑥 10−6 was obtained. It was
𝐿−𝑠

also observed that as time passes by, the presence

of the product interferes with the reaction resulting in
discrepancies in the second order reaction.
REFERENCES

1. Edibon. (2012). Practical Exercises Manual.

2. Fogler, H.S. (2004). Elements of Chemical
Reaction Engineering (3rd ed.). New Delhi:
PrenticeHall India.
3. Ullah, I., Ahmad, M. I., Younas, M. (2015).
Optimization of saponification re9action in a
continuous stirred tank reactor (CSTR) using
design of experiments. Pakistan Journal of
Engineering and Applied Science, 16, 84-92.