Results and analysis

Table 1 – Preparation of Calibration Curve for Conductivity vs. Conversion

Conversion Solution Mixtures Concentration Conductivity

(%) 0.1 mol/L 0.1 mol/L Deionised of NaOH (mS/cm)
NaOH (mL) Et(Ac) (mL) water (mL) (mol/L)

0 100 - 100 0.0500 7.31

25 75 25 100 0.0375 5.07
50 50 50 100 0.0250 2.83
75 25 75 100 0.0125 1.80
100 - 100 100 0.0000 0.04

Conductivity vs. Conversion of NaOH

8
f(x) = − 1.78 x + 10.53
7

6
Conductivity (mS/cm)

0
0 1 2 3 4 5 6 7
Conversion of NaOH (%)

Conductivity (mS/cm) Linear (Conductivity (mS/cm))

Fig. 1 - Conductivity against Conversion of Calibration Curve

 Table 2 – Effect of Residence Time of the Reaction in a CSTR

Flowrate of NaOH (L/min) 0.10 0.15 0.20 0.25 0.30

Flowrate of Et (Ac) (L/min) 0.10 0.15 0.20 0.25 0.30

Temperature (°C) 28.6 28.6 28.8 28.9 29.0

Conductivity (mS/cm) 3.11 3.12 3.13 3.14 3.16

Volume of NaOH titrated, V1 (mL) 18.5 17.5 19.8 19.1 19.1

Residence time, τ (min) 50.0 33.33 25.00 20.00 16.67

Volume of unreacted quenching HCl, 7.40 7.00 7.92 7.64 7.64

V2 (mL)
Volume of HCl reacted with NaOH, 2.60 3.00 2.08 2.36 2.36
V3 (mL)
Concentration of unreacted NaOH in 0.013 0.015 0.0104 0.0118 0.0118
the reactor, CNaOH (mol/L)
Conversion of NaOH in the reactor, 74.0 70.0 79.2 76.4 76.4
X (%)
Rate constant, k (L/mol.s) 0.0730 0.0778 0.2441 0.2286 0.2743

Rate of reaction, -rA (mol/L.s ) 1.23 x 10-5 1.75 x 10-5 2.64 x 10-5 3.18 x 10-5 3.82 x 10-5
 Conversion of NaOH vs. Residence Time
80

78

76 f(x) = − 0.13 x + 78.85

Conversion of NaOH (%)

74

72

70

68

66

64
15 20 25 30 35 40 45 50 55
Residence Time, τ (min)

Conversion of NaOH in the reactor, X (%)

Linear (Conversion of NaOH in the reactor, X (%))

Fig. 2 – Graph of Effect of Residence Time on the Conversion of NaoH

Conversion, X
0.8

0.78

0.76

0.74

0.72

0.7

0.68

0.66

0.64
15 20 25 30 35 40 45 50 55

Sample of calculation
For flowrate of NaOH = flowrate of Et (Ac) =0.10 L/min
 Volume of sample, Vs 50 mL
Concentration of NaOH in the feed vessel, 0.1 M
CNaOH,f
Volume of HCl for quenching, VHCl,s 10 mL
Concentration of HCl in standard solution, 0.25 M
CHCl,s
Volume of NaOH titrated, V1 18.5
Concentration of NaOH used for titration, 0.1 M
CNaOH,s

1. Concentration of NaOH entering the reactor, CNaOHo

CNaOHo = (1/2) (CNaOH,f)

= (1/2) (0.1)

= 0.05 mol/L

2. Volume of unreacted quenching HCl, V2

V2 = (CNaOHs, / CHCl,s) x V1

= (0.1/0.25) x 18.5

= 7.4 mL  placed in Table 1

3. Volume of HCl reacted with NaOH in sample, V3

V3 = VHCl,s –V2

= (10-7.4) mL

= 2.6 mL  placed in Table 1

4. Moles of HCl reacted with NaOH in sample, n1

n1 = (CHCls x V3) / 1000

= (0.25 x 2.6) /1000

= 0.00065 mol
 Moles of unreacted NaOH in sample, n2 = n1 = 0.00065 mol

5. Concentration of unreacted NaOH in the reactor, CNaOH

CNaOH = n2 / Vs x 1000

= 0.00065 / 50 x 1000

= 0.013 mol/L

6. Conversion of NaOH in the reactor, X

C NaOH
X = 1−( C NaOH , 0)× 100 %

0.013
= 1−( 0.05 )
× 100 %

= 74.0 %  Placed in Table 1

7. Residence time, τ

τ = VCSTR / V0

= 10L / (0.10 + 0.10) L/min

= 50 min  placed in Table 1

8. Rate constant, k

(C ¿ ¿ NaOH , 0−C NaOH )

k ¿ ¿
tC 2NaOH

0.05−0.013
¿
¿¿

= 4.3787 L/mol.min
 = 0.0730 L/mol.s

9. Rate of reaction, -rNaOH

-rNaOH = kCNaOH2 = 0.0730 (0.013)2 = 1.23 x 10-5 mol/L.s  placed in Table 1

The calculation of these nine values were repeated for other flowrates and tabulated in
Table 1.

Analysis

The calibration curve was prepared for conductivity versus conversion of NaOH as
shown in Fig. 1. The graph shows that the conductivity is inversely proportional with the
conversion. As the conversion of NaOH increases, the conductivity decreases. The amount of
conversion indicates the concentration of NaOH left in the solution mixtures as shown in Table
1. As the conversion increases, the concentration of NaOH left decreases. Thus, results in the
decrease of conductivity value.

Experiment 1 was conducted to determine the effect of residence time on the conversion
of NaOH. The graph in Fig. 2 was plotted according to the value of residence time and
conversion of NaOH calculated after the experiment and was tabulated in Table 2. The plot
shows that the the conversion increase from 16.67 min to 25 min residence time and the
conversion decrease with residence time from 25 min to 33.3 min residence time and the
conversion increase back from 33.3 min to 50 min which were quite insignificant trend pattern
where chemical reactant that should be used up more at a longer residence time. Theoretically,
the amount of conversion should be increase with the residence time. This error occurs probably
due to the mistake while doing the back titration because the volume of NaOH titrated was used
for the calculation to obtain the value of conversion for each flowrate. The volume of NaOH
titrated should increase with the residence time in order to obtain the right amount of conversion.
The value of rate constant, k was determined after the value of residence time and C NaOH was
obtained.
Conclusions

From experiment, the reaction yield conversion of 76.4%, 76.4%, 79.2% and 74% for
residence time of 16.67-minute, 20-minute, 25-minute, 33-minute and 50-minute. It shows that
the conversion increase from 16.67 min to 25 min residence time and the conversion decrease
with residence time from 25 min to 33.3 min residence time and the conversion increase back
from 33.3 min to 50 min. The pattern trend of conversion over residence time were unacceptable
because more conversion should be achieve for a longer residence time. This fluctuation is due to
poor back-titration analysis in order to determine the concentration of NaOH at a residence time
or also might cause by inconsistency of reactor mixing condition.

From results, we also can relate the conductivity with conversion from this experiment. The
conductivity of a solution decreases as the conversion are increases which indicates the
concentration of NaOH in reactor vessel decreases as it consumed in the reaction.

Recommendations

Accurate observation on titration endpoint will give you the correct amount of chemical
present in sample. The ‘light pink’ color indicator for all titrate sample should standardize its
intensity and the correct one is when a ‘very light pink’ color formation. Observe the color
intensity of titrate solution on white tiles for better sight. Excess drop of titrant into titrate sample
will cause drastic changes of indicator color. Small drop of titrant is preferable when approach
titration endpoint. Avoid parallax error when measure the volume of titrant in the burette. Make
sure the level of CSTR vessel is maintain at 10 Liter in order to get the desired residence time.

References

Continuous Stirred Tank Reactor 40L. Retrieved October 23, 2019 from
https://www.scribd.com/document/179119924/CSTR-40L-docx

Md Tahir, N. S, (September, 2018). Retrieved October 23, 2019 from

file:///C:/Users/User/Downloads/Lab_Report_Tubular_Flow_Reactor.pdf