Experiment #3

Isothermal Reaction in a Plug Low Tubular Reactor

Date Performed: Jan. 20, 1014

Date Submitted: Feb. 4, 2014

Submitted by:
Cansana, Benedicto III
Gomez, Rainer
Holaysan, Sed
Kato, Yuji

Submitted To:
Dr. Kathleen Aviso
 I. Data

(A) Initial Concentration of NaOH (mol/ml) 0.00005

(B) Initial Concentration of EtAc (mol/ml) 0.00005
Concentration of NaOH titrant (mol/ml) 0.0001
Concentration of HCL (mol/ml) 0.000089

Part II: Varying Flow Rate

A. Ambient Temperature for Part II (deg C) 26

Run 1
Ethyl Acetate Flow Rate (ml/min) 30
NaOH Flow Rate (ml/min) 30
Final Volume
Time (min) Initial Volume (ml) (ml) Volume of Titrant Used (ml)
5 12.8 20.9 8.1
10 20.9 28.6 7.7
Average Volume of Titrant Used (ml) 7.9

Run 2
Ethyl Acetate Flow Rate (ml/min) 40
NaOH Flow Rate (ml/min) 30
Final Volume
Time (min) Initial Volume (ml) (ml) Volume of Titrant Used (ml)
5 28.6 37.6 9
10 37.6 46.3 8.7
Average Volume of Titrant Used (ml) 8.85

Run 3
Ethyl Acetate Flow Rate (ml/min) 40
NaOH Flow Rate (ml/min) 40
Final Volume
Time (min) Initial Volume (ml) (ml) Volume of Titrant Used (ml)
5 10 18 8
10 18 26.3 8.3
Average Volume of Titrant Used (ml) 8.15
Part III: Varying Temperature

Run 1
Operating Temperature(deg C) 33
Ethyl Acetate Flow Rate (ml/min) 30
NaOH Flow Rate (ml/min) 30
Final Volume
Time (min) Initial Volume (ml) (ml) Volume of Titrant Used (ml)
5 26.3 34.6 8.3

Run 2
Operating Temperature(deg C) 40
Ethyl Acetate Flow Rate (ml/min) 30
NaOH Flow Rate (ml/min) 30
Final Volume
Time (min) Initial Volume (ml) (ml) Volume of Titrant Used (ml)
5 34.6 43.2 8.6

II. Data Analysis

For varying volume

Run Ca (mol/ml) Xa (% conversion) Space time (min) k

1 3.68333E-05 26.33333333 6.666667 1072.398

2 3.73571E-05 25.28571429 5.714286 1184.512

3 3.98125E-05 20.375 5 1023.548

 % Conversion Vs. Space Time (min)
30

25
% Conversion
20

15

10

0
0 1 2 3 4 5 6 7 8
Space Time (min)

For varying temperature

*data from run 1 is taken from run 1 of varying volume for the temperature of 26 deg C

Run Ca (mol/ml) Xa (% conversion) Space time (min) k

1 3.68333E-05 26.33333333 6.666667 1072.398

2 3.61667E-05 27.66666667 6.666667 1147.465

3 3.56667E-05 28.66666667 6.666667 1205.607

Eq: log k = -(E/R)(1/T) +

log A
Run log K 1/T
1 3.0304 3.3440 E-03
2 3.0597 3.2680 E-03
3 3.0812 3.1949 E-03

E A
0.02424 J 1.028
Estimating the order of reaction
*using runs from varying volume

Run ln Cao/Ca Timespace

1 0.30762 6.667
2 0.2915 5.7143
3 0.2278 5
R2 0.8381

Run 1/Ca Timespace

1 27149.57 6.667
2 26768.67 5.7143
3 25117.74 5
R2 0.8270

Run Ca0.5 Timespace

1 6.069 E-03 6.667
2 6.112 E-03 5.7143
3 6.3097 E-03 5
R2 0.8190

Estimated order of reaction: n =1

 III. Results

For the first analysis in which the values of the % conversion were plotted against space time
for the varying flow rate trials, % conversion increases as space time increases. The reason
behind this is that for a larger space time, the reactants have more time in reacting, thus,
producing more products. It was also observed that the highest % conversion is achieved when
the total flow rate is lower and its reason is due to its effect on space time (lower total flow rate
leads to a higher space time, thus, a higher % conversion). From the varying temperature trials,
as temperature increases (keeping space time constant), the % conversion increases.

The determination of the reaction constant k was done under the assumption that the reaction
had an order of 2. Knowing this, the values of k for both varying flow rate and varying
temperature were solved. To plot the concentration against residence time was then unnecessary.
The relationship of k with respect to % conversion varies as there were no such trends seen in the
data gathered.

The Arrhenius constants A and E were calculated from the varying temperature trials. The
activation energy was calculated to be 0.02424 J and has a frequency factor of 1.028.

To estimate the order of reaction, 3 orders of 1, 2, and 1.5 were put under trial. Using the
values from the varying flow rate trials, the R squared values for the equation of the lines for
each order were determined. Upon the results, the highest R squared value will decide the order
of the reaction. Thus, the order of the reaction is estimated to be 1.

Other than manual titration, a more efficient way is the use of an automatic titration system.
The HI 901 Automatic Titration System by Hanna instruments can support up to 10, 000
methods which can be standard or user define and all the data including the graph at the end of
the titration are automatically stored in memory and can be transferred from port to port via cable
or USB. Because it is automated, it is faster and more accurate as compared to the manual
methods, though the only drawback here is the knowledge on equipment and the price of the
equipment itself.

IV. Conclusion

The experiment was done with all analyses completed. As the total flow rate increases, the
space time decreases. As space time decreases, % conversion also, decreases. As temperature
increases, % conversion also, increases. K values are highly empirical and can have no trends.
The activation energy was calculated to be 0.02424 J and has a frequency factor of 1.028. The
order of the reaction is 1. The only recommendation for this experiment is to use a more accurate
method in determining the concentration of the products like the use of an automatic titration
system.