CHEE3005: EXPERIMENT 1

1. AIM AND OBJECTIVES OF THE EXPERIMENT

The main objective of practical session 1 is to demonstrate the working of 3 ideal reactors, which
are batch reactor, continuous stirred tank reactor (CSTR) and plug flow reactor (PFR). The team
has been allocated to investigate the conversion in a CSTR. In which, the team is to collect and
analyse the experimental data obtained from the assigned reactor.
For this CTSR experiment, the effect of the feed flow rate as an input parameter on the reactor
performance is to be explored. This led to the estimation of the reactor’s performance by
measuring the conversion of an equimolar 2nd order reaction.
All the three different reactor experiments are based on the same saponification reaction between
sodium hydroxide and Ethyl Acetate. In this saponification reaction, the hydrolysis of Ethyl
Acetate in the presence of sodium hydroxide will produce Sodium Acetate and Ethyl Alcohol.
NaOH + CH3COOC2H5 -> CH3COONa +
C2H5OH A + B -> C
+ D
Hence, specifically, the team is to investigate the effect of reactants’ flow rate (space time) on
the conversion of sodium hydroxide (NaOH, reactant A) when being reacted with Ethyl Acetate
(CH3COOC2H5, reactant B). The team has conducted the experiment at three different flow rates
(space times) of reactants; 50 ml/min, 60 ml/min and 70 ml/min. The experimental data has been
analysed to obtain the conversion in a CTSR. Also, the team has performed the calculation of the
conversion in the other two reactors, batch reactor and PFR, theoretically. This followed by a
discussion on the conversion performance across the three different reactors.

2. EXPERIMENTAL PROCEDURE
Stirrer

CSTR tank

Reagent tank for

sodium hydroxide Drain valve

Reagent tank for

Ethyl Acetate

Temperature reading

Hot water flow tube Conductivity reading

connected to water

Stirrer control

Pump 1 dial
Power supply switch
Pump 1 control

Pump 2 dial

Pump 2 control
Figure 1: Experiment set up (Source: CHEE3005 Reaction Engineering Practical_1)
1
 The rig for a CSTR experiment is set-up as shown in Figure 1. Initially, the electrical supply to
the rig is ensured to be turned off and the reactor tank is emptied and cleaned. The reagent tanks
for sodium hydroxide and Ethyl Acetate are checked to have sufficient volume. While the pumps
and stirrer control are switched off (put to remote mode) and the drain valve of the reactor is
ensured to be closed, before switching on the power supply of the rig. To control the reaction
temperature, a water bath is used and set to 30oC. It is connected to the reactor through the hot
water flow tube.
Each of the reactant pumps, pump 1 (Ethyl Acetate) and pump 2 (sodium hydroxide), are set to
50 ml/min by turning the dial next to the pump control. The calibration of the dial number and
the flow rate is calculated using the given calibration graph for each pump that are provided in
the Lab Manual.
Next, the pumps are switched on (put to manual mode) together to allow the reactor tank to be
filled with reactants, sodium hydroxide and Ethyl Acetate, at flow rates of 50 ml/min each. The
reactor filling is observed until it is half-filled where the stirrer will need to be switched on.
Then, the reactor is further be observed for it to be full-filled, which indicated by the presence of
reactants dripping out of the reactor from the bottom of the tank.
Once the reactor is full-filled, the data on time, conductivity and temperature are recorded for
every 2 minutes until the conductivity reached a constant value. Then, the pumps and stirrer
control are switched off (put to remote mode). The product from the reactor is drained using the
drain valve.
The experiment is repeated for different flow rates of reactants, which are at 60 ml/min and 70
ml/min. Once all the three experiment’s run are completed, the rigs power supply is switched off
and both the conductivity probe and the stirrer are carefully rinsed with clean water.

3. RESULTS
3.1. Table of results

Reactor volume = 1600 mL

CA0 = CB0 = 0.05 M
Table 1: Residence time for required flow rates for the reactor volume of 1600 mL.

Flow rates of each Total flow rates Residence time

reactant (mL/min) (mL/min) (min)

50.0 100.0 16.0

60.0 120.0 13.0
70.0 140.0 11.0

Table 2: Calculated and experimental data for CSTR

Flow rates of each Total flow Space time Calculated Experimental

reactant (mL/min) rates (min) XA XA
(mL/min)
50.0 100.0 16.0 0.696 0.720
60.0 120.0 13.0 0.672 0.694
70.0 140.0 11.0 0.650 0.677
Table 3:Calculated data for Batch Reactor and PFR using the same space time as in CSTR

Space Batch Reactor PFR

time
XA XA
(min)

16.0 0.887 0.887

13.0 0.864 0.864
11.0 0.843 0.843

3.2. Plot of Conversion of CSTR against Space Time

Conversion A in CSTR versus Space Time

0.75

0.7
Conversion, XA

0.65

Calculated XA
0.6 Measured XA

0.55

0.5
10.011.012.013.014.015.016.017.0
Space time (min)

Plot 1: Graph of conversion against space time.

3.3. Sample Calculation of Conversion for CSTR (flow rate 50 mL/min)

 Initial concentration, CA0 using dilution equation

M1V1 = M2V2
M1 = MA = 0.1M
V1 = VA = 500 mL = 0.5 L
V2 = VA + VB = 500 mL + 500 mL = 1 L
0.1 M(0.5 L) = M2(1 L)

M2 = 0.05 M = CA0 = CB0

 Space time/Residence time using Equation 8
Volume of reactor V
τ= =
Volumetric flowrate ν
1600 mL
τ =
100 mL/min
τ = 16 minutes

 Change unit of conductivity

conductivity = 5.54
mS 10−3 = 0.00554 S
1m cm
×
cm

 Rate constant was calculated from graph ln K vs 1/T

y = mx + C
y = ‐ 5010.6x + 18.818
ln k = ‐ 5010.6 (1/T) + 18.818
k = exp (5010.6 × (1/302.05) + 18.818)
k = 9.294 (L/mol. min)

 Outlet concentration using Equation 5

0.00975 − conductivity
C A = CA0 – CA0
0.00975 − 0.0035
0.00975 − 0.00554
CA = 0.05 – 0.05
0.00975 − 0.0035
CA = 0.01632 mol/L

 Conversion measured using Equation 4

𝑋𝐴 = CA0C– CA
A0

0.5 − 0.01632
𝑋𝐴 =
0.5
𝑋𝐴 = 0.674

 Calculated conversion using Equation 10

XA
𝜏=
kCA0(1 − XA)2
τkCA0(1 − XA)2 = X

τkCA0 − 2τkCA0XA + τkCA0X2 =

A X

τkCA0 − (2τkCA0+1) XA + τkCA0X2 =

A 0
 −b±√b −4ac
Using quadratic formula: X = 2
2a

− (−2τkCA0 − 1) ± √(−2τkCA0 − 1)2 − 4(τkCA0)(τkCA0)

XA =
2(τkCA0)

(2τkCA0 + 1) ± √(4τkCA0 + 1
X A= 2τkCA0

XA = (2 × 16 × 9.294 × 0.05 + 1) ± √(4 × 16 × 9.294 × 0.05) + 1

2 × 16 × 9.294 × 0.05
XA = 0.694 and 1.440
∴ XA = 0.694

3.4. Sample Calculation of Conversion for Batch Reactor

Using the formula : (1−𝑋𝐴)

𝑋𝐴
= 𝑘. 𝐶𝐴𝑜. 𝑡
𝑘.𝐶𝐴𝑜.𝑡
Rearranging the formula : 𝑋𝐴 =
1+𝑘.𝐶𝐴𝑜.𝑡

Calculation at t = 16 min,
k = 9.7805 L mol-1 min-1
CAO = 0.05 M
t = 16 min

9.7805 L mol−1 min−1 × 0.05 𝑀 × 16 𝑚𝑖𝑛

Conversion/XA = 1+ (9.7805 L mol−1 min−1 × 0.05 𝑀 × 16 𝑚𝑖𝑛)

= 0.887

3.5. Sample Calculation of Conversion for PFR

𝑋𝐴
Using the formula :=
𝑘.𝐶𝐴𝑂.(1−𝑋𝐴)
.𝑘.𝐶𝐴𝑜
Rearranging the formula : 𝑋𝐴 =
1+𝑘.𝐶𝐴𝑜.

Calculation at t = 16 min,
k = 9.7805 L mol-1 min-1
CAO = 0.05 M

 = 16 min

16 min × 9.7805 L mol−1 min−1 × 0.05 𝑀

Conversion/XA = 1+ (9.7805 L mol−1 min−1 × 0.05 𝑀 × 16 𝑚𝑖𝑛)

= 0.887
4. DISCUSSIONS (error analysis)

Saponification reaction kinetics studies in this experiment were run at constant volume tank reactor
(1600 ml), stirring rate and temperature and variable of feed flow rates. Based on the results section
above, conversion of sodium hydroxide (NaOH) in saponification reaction between Ethyl acetate
(CH3COOC2H5) to produce Sodium Acetate (CH 3COONa) and Ethyl Alcohol (C2H5OH) in
continuous stirred tank reactor (CSTR) is greatly affected by the feed flow rate and space time. By
referring to Table 2, feed flow rate shows an inversely proportional relationship to the conversion of
NaOH, whose total feed flow rates of 100 ml/min, 120 ml/min and 140 ml/min gives conversion of
0.72, 0.69 and 0.68 respectively. Apart from that, space time which the time necessary to process
one reactor volume of fluid based on inlet conditions shows a linear relationship to the conversion
of NaOH. This can be seen based on the values obtained whose 16 min, 13 min and 11 min give
0.72,
0.69 and 0.68 conversion of NaOH respectively. The comparison between experimental data and
theoretically calculated data are the same trends for both factors, total reactant flow rate and space
time, that affecting the NaOH conversion. Previous studies on effect of operating conditions on
CSTR performance stated that conversion is decreasing as flow rate increase, this is due to the
depletion of residence time by means the higher reactants flow rates not consistently desirable for
practical application, whose the reactants flow rate of 40 ml/min, 50 ml/min and 60 ml/min gives
0.54, 0.52 and 0.49 total conversion of NaOH respectively (Danish, Al Mesfer, & Rashid, 2015).
Based on Plot 1, it can be deduced that the effect of reactants flow rate and space time with respect
to the experimental conversion are similarly to the literature.
Next, theoretical values obtained for NaOH conversion are the same for both batch and plug flow
reactor (PFR) based on space time where 16 min, 13 min and 11 min gives 0.887, 0.864 and 0.843
respectively but slightly different compared to CSTR. Effect of flow rate and space time for both
PFR and CSTR shows that as space time (residence time) decreases and the feed flow rate is
increases resulting to decrease values of conversion (M. K. Al Mesfer & Danish, 2015).
Furthermore, PFR gives higher conversion compared to the CSTR due to the reaction rate
concentration and sizes of volume. Technically, CSTR has a larger volume tank and mode of axial
mixing compared to the PFR depends on radial mixing mode by means CSTR converting the
reactants in shorter time than PFR (Shinde, 2015). As for batch reactor, the conversion of NaOH is
highly dependent on the reaction time (holding time). According to (M. K. A. Mesfer, 2018),
relationship between NaOH conversion is linear to the retention time until the stable condition is
achieved. To sum up, conversion of NaOH in saponification reaction is affected by volume reactor
tank, temperature, stirring speed and mode, feed flow rate and space time for the continuous reactor,
reaction in batch somehow is affected by the same factors except for the feed flow rate.
The significant difference between experimental and theoretically conversion of NaOH might came
from the errors introduced in the experimental data. One of the sources for random error is the
experimenter’s observation in recording the conductivity data for every 2 minutes. This leads to
possible inaccuracy of conductivity data and hence affects the experimental conversion of NaOH.
Another source of error might contribute by the environmental factor during conducting the
experiment. Throughout the duration of experiment for each flow rate, the temperature inside the
CSTR are slightly varied (refer to table of data in Appendix). This factor might has affected the rate
of conversion rate in the CSTR for all three experiments run. Also, the experimental data might be
inaccurate due to instrument errors that came from the temperature probe, conductivity probe or
feed pumps used. Only the feed pumps have been calibrated in this experiment, but not temperature
probe and conductivity probe. These might lead to error in reading the temperature and conductivity
data obtained.
5. SUMMARY AND CONCLUSION

The performance of different reactors which are CSTR, batch reactor and PFR, have been explored
in this experiment by measuring the conversion of sodium hydroxide (NaOH) in saponification
reaction. For CSTR, both experimental and theoretical conversion of NaOH obtained shows similar
trends which are the conversion of NaOH is inversely proportional with the total flow rate of
reactants, but it is directly proportional to the space time (residence time). This outcome agrees with
the prediction from a literature that confirms the conversion is decreasing as flow rate increase due
to the depletion of residence time. However, the significant difference in the experimental and
theoretical value of conversion in CSTR might have been contributed by the low accuracy of
experimental data.
Next, it is found that the theoretical NaOH conversions for batch reactor and PFR, using the same
space time as in the CSTR experiment, are similar in values and show the same trend as in CSTR;
conversion is directly proportional to the space time. However, in comparison to CSTR, both batch
reactor and PFR have a higher conversion of NaOH at a particular space time. For PFR, the reason
behind this is because technically, CSTR has a larger volume tank and mode of axial mixing
compared to the PFR. Hence, CSTR converting the reactants in shorter time than PFR and resulting
in lower conversion for CSTR compared to PFR. Meanwhile for batch reactor, the conversion of
NaOH is highly dependent on the reaction time (holding time). So, for a particular space time, the
saponification reaction takes place in batch reactor has a higher reaction rate and hence the obtained
a higher conversion of NaOH, compared to in CSTR.
In conclusion, the conversion of NaOH in saponification reaction is affected by both feed flow rate
and space time for all different type reactors. Other factors that also affects the conversion
depending on the type of reactors used are volume of the reactor tank, temperature and stirring
speed and mode.
6. REFERENCES

Al Mesfer, M. K., & Danish, M. (2015). A Comparative Study of Saponification Reaction in a PFR and
CSTR. Research Journal of Chemical Sciences, 5(11), 13–17. Retrieved from www.isca.me
Danish, M., Al Mesfer, M. K., & Rashid, M. (2015). Effect of Operating Conditions on CSTR performance:
an Experimental Study. Journal of Engineering Research and Applications, 5(2), 74–78. Retrieved
from https://www.ijera.com/papers/Vol5_issue2/Part - 2/K502027478.pdf
Mesfer, M. K. A. (2018). Experimental Study of Batch Reactor Performance for Ethyl Acetate
Saponification. International Journal of Chemical Reactor Engineering, 16(1).
https://doi.org/10.1515/ijcre-2016-0174
Shinde, P. (2015). For the same volume, which reactor has the highest conversion, a CSTR or a PFR?
Why? Retrieved September 6, 2019, from https://www.quora.com/For-the-same-volume-which-
reactor-has- the-highest-conversion-a-CSTR-or-a-PFR-Why
 7. APPENDIX
Table 4:Data for flow rate 50.0 mL/min.

T T (K) Time Conductivity Conductivity k Outlet Calculated Measured

(˚C) (min) (mS/cm) (S/cm) (L/mol.min) concentration, XA XA
CA (mol/L)

28.9 302.05 0.0 5.54 0.00554 9.294 0.01632 0.694 0.674

28.9 302.05 0.5 5.51 0.00551 9.294 0.01608 0.694 0.678

29.0 302.15 1.0 5.47 0.00547 9.345 0.01576 0.695 0.685
29.0 302.15 1.5 5.43 0.00543 9.345 0.01544 0.695 0.691
29.0 302.15 2.0 5.40 0.00540 9.345 0.01520 0.695 0.696
29.0 302.15 2.5 5.38 0.00538 9.345 0.01504 0.695 0.699
29.0 302.15 3.0 5.36 0.00536 9.345 0.01488 0.695 0.702
29.0 302.15 3.5 5.34 0.00534 9.345 0.01472 0.695 0.706
29.0 302.15 4.0 5.32 0.00532 9.345 0.01456 0.695 0.709
29.1 302.25 4.5 5.31 0.00531 9.396 0.01448 0.696 0.710
29.1 302.25 5.0 5.30 0.00530 9.396 0.01440 0.696 0.712
29.1 302.25 5.5 5.29 0.00529 9.396 0.01432 0.696 0.714
29.1 302.25 6.0 5.28 0.00528 9.396 0.01424 0.696 0.715
29.1 302.25 6.5 5.27 0.00527 9.396 0.01416 0.696 0.717
29.1 302.25 7.0 5.27 0.00527 9.396 0.01416 0.696 0.717
29.1 302.25 7.5 5.26 0.00526 9.396 0.01408 0.696 0.718
29.1 302.25 8.0 5.25 0.00525 9.396 0.01400 0.696 0.720
29.1 302.25 8.5 5.25 0.00525 9.396 0.01400 0.696 0.720
29.1 302.25 9.0 5.25 0.00525 9.396 0.01400 0.696 0.720
 Table 5: Data for flow rate 60.0 mL/min.

T T (K) Time Conductivit Conductivit k Outlet Calculate Measured

(˚C (min y (mS/cm) y (S/cm) (L/mol.min concentration, CA d XA XA
) ) ) (mol/L)
28.7 301.85 0.0 5.71 0.00571 9.192 0.01768 0.669 0.646

28.8 301.95 0.5 5.66 0.00566 9.243 0.01728 0.670 0.654

28.8 301.95 1.0 5.61 0.00561 9.243 0.01688 0.670 0.662
28.8 301.95 1.5 5.58 0.00558 9.243 0.01664 0.670 0.667
28.8 301.95 2.0 5.55 0.00555 9.243 0.01640 0.670 0.672
28.9 302.05 2.5 5.52 0.00552 9.294 0.01616 0.671 0.677
28.9 302.05 3.0 5.50 0.00550 9.294 0.01600 0.671 0.680
28.9 302.05 3.5 5.48 0.00548 9.294 0.01584 0.671 0.683
28.9 302.05 4.0 5.46 0.00546 9.294 0.01568 0.671 0.686
28.9 302.05 4.5 5.45 0.00545 9.294 0.01560 0.671 0.688
28.9 302.05 5.0 5.44 0.00544 9.294 0.01552 0.671 0.690
29.0 302.15 5.5 5.43 0.00543 9.345 0.01544 0.672 0.691
29.0 302.15 6.0 5.42 0.00542 9.345 0.01536 0.672 0.693
29.0 302.15 6.5 5.41 0.00541 9.345 0.01528 0.672 0.694
29.0 302.15 7.0 5.41 0.00541 9.345 0.01528 0.672 0.694
29.0 302.15 7.5 5.41 0.00541 9.345 0.01528 0.672 0.694
 Table 6: Data for flow rate 70.0 mL/min.

T T (K) Time Conductivity Conductivity k Outlet Calculated Measured

(˚C) (min) (mS/cm) (S/cm) (L/mol.min) concentration, XA XA
CA (mol/L)

28.5 301.65 0.0 5.98 0.00598 9.092 0.01984 0.647 0.603

28.6 301.75 0.5 5.90 0.00590 9.142 0.01920 0.648 0.616

28.6 301.75 1.0 5.84 0.00584 9.142 0.01872 0.648 0.626
28.7 301.85 1.5 5.74 0.00574 9.192 0.01792 0.649 0.642
28.7 301.85 2.0 5.72 0.00572 9.192 0.01776 0.649 0.645
28.7 301.85 2.5 5.70 0.00570 9.192 0.01760 0.649 0.648
28.8 301.95 3.0 5.68 0.00568 9.243 0.01744 0.649 0.651
28.8 301.95 3.5 5.65 0.00565 9.243 0.01720 0.649 0.656
28.8 301.95 4.0 5.63 0.00563 9.243 0.01704 0.649 0.659
28.8 301.95 4.5 5.61 0.00561 9.243 0.01688 0.649 0.662
28.8 301.95 5.0 5.59 0.00559 9.243 0.01672 0.649 0.666
28.9 302.05 5.5 5.58 0.00558 9.294 0.01664 0.650 0.667
28.9 302.05 6.0 5.57 0.00557 9.294 0.01656 0.650 0.669
28.9 302.05 6.5 5.56 0.00556 9.294 0.01648 0.650 0.670
28.9 302.05 7.0 5.55 0.00555 9.294 0.01640 0.650 0.672
28.9 302.05 7.5 5.54 0.00554 9.294 0.01632 0.650 0.674
28.9 302.05 8.0 5.53 0.00553 9.294 0.01624 0.650 0.675
28.9 302.05 8.5 5.53 0.00553 9.294 0.01624 0.650 0.675
28.9 302.05 9.0 5.52 0.00552 9.294 0.01616 0.650 0.677
28.9 302.05 9.5 5.52 0.00552 9.294 0.01616 0.650 0.677
28.9 302.05 10.0 5.52 0.00552 9.294 0.01616 0.650 0.677