DEPARTMENT OF CHEMICAL AND ENVIRONMENTAL ENGINEERING

ECH 3905
CHEMICAL ENGINEERING LABORATORY III
LAB REPORT
EXPERIMENT 1 : MEASURING THE CHEMICAL REACTION IN CONTINUOUS
STIRRED TANK REACTOR (CSTR)
EXPERIMENT 2 : EXPERIMENT 2: EFFECT OF MIXING SPEED ON
REACTION RATE CONSTANT

LECTURER’S NAME : DR. MUHAMAD FAIZ MUKHTAR BIN GUNAM RESUL

SUBMISSION DATE : 3 JULY 2020
GROUP 7
1. NUR A'INA SHAFIQA BINTI WAKARI 194892
2. OOI SHU WEN 194190
3. DIVAGAR A/L SIVASELVAM 194893
4. HARIHARAN A/L DEVARAJ 194895
5. MAHFUZ ALAM 195405

1
Abstract

A continuous stirred tank reactor (CSTR) is a reactor equipped with an impeller or

other mixing device to provide efficient mixing. The impeller stirs the reagents to ensure
proper mixing of the reactants that enter the CSTR. All calculations performed on this CSTR
is assumed to be perfect mixing thus the output composition of the reactor is identical to the
composition of material inside the reactor. In this experiment the first part is to identify the
order of saponification reaction between ethyl acetate and sodium hydroxide to produce
sodium acetate and ethanol and also the reaction rate constant. The feed concentration is 5 L
of 0.05 M NaOH and 5 L of 0.05 M EtOAc, with the mixing speed of 4.5 rpm for the first
experiment. The mixing speed is kept unchanged for the first experiment. Based on the data
of this experiment when the sampling time increases, the concentration of unreacted NaOH
decreases. This saponification reaction has overall second order reaction with the rate
constant of 66.873 M-1·min-1. For this second experiment, the effect of mixing speed is
studied. The feed concentration is kept constant and speed of the impeller is set at 1.5rpm,
4.5rpm and 6.5rpm. The higher the speed of mixing the higher the rate of reaction.

2
Results

Volume of Volume of quenching Volume of HCl Mole of HCl

Sampling
tirating HCl unreacted with reacted with NaOH reacted with
time (min)
NaOH (mL) NaOH in sample (mL) in sample (mL) NaOH in sample

1 21.6 8.64 1.36 0.000340

5 22 8.80 1.20 0.000300
10 24.3 9.72 0.28 0.000070
15 24.5 9.80 0.20 0.000050

Table 1. Data obtained for different sampling time.

Steady State
Concentration of Concentration of
Mole of NaOH Fractional
NaOH unreacted with NaOH reacted with
unreacted in sample Conversion of
ethyl acetate (M) ethyl acetate (M)
NaOH
0.000340 0.00680 0.04320 0.864
0.000300 0.00600 0.04400 0.880
0.000070 0.00140 0.04860 0.972
0.000050 0.00100 0.04900 0.980

Table 2 Calculated data for different sampling time.

Sampling time
ln(CA) 1/CA 1/CA2
(min)
1 -4.991 147.059 1.340
5 -5.116 166.667 1.291
10 -6.571 714.286 1.058
15 -6.908 1000.000 1.041

Table 3: Data for Graph plotting to determine the reaction order.

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 ln (CA) VS Time
0
-1 0 2 4 6 8 10 12 14 16

-2
-3
y = -0.1545x - 4.6992
ln (CA)
-4 R² = 0.9092
-5
-6
-7
-8
Time (min)

Figure 1. Graph of ln (CA) versus Time

1/CA VS Time y = 66.873x - 11.261

R² = 0.932
1200
1000
800
1/CA

600
400
200
0
0 2 4 6 8 10 12 14 16
Time (min)

Figure 2. Graph of 1/CA versus Time

1/CA2 VS Time
1.6
1.4
1.2
1
1/CA2

0.8 y = -0.0241x + 1.3692

0.6 R² = 0.8911
0.4
0.2
0
0 2 4 6 8 10 12 14 16
Time (min)

Figure 3. Graph of 1/CA2 versus Time

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 Volume of
Volume of Mole of Concentration
Volume quenching Mole of
Samplin HCl reacted NaOH of NaOH
of NaOH HCl HCl reacted
g time with NaOH unreacte unreacted
used unreacted with NaOH
(min) in sample d in with ethyl
(mL) with NaOH in in sample
(mL) sample acetate (M)
sample (mL)
0 19.5 7.80 2.20 0.000550 0.000550 0.01100
5 20.3 8.12 1.88 0.000470 0.000470 0.00940
10 22.5 9.00 1.00 0.000250 0.000250 0.00500
15 23.2 9.28 0.72 0.000180 0.000180 0.00360

Table 4. Data obtained for impeller speed at 1.5 rpm.

Volume of Volume of Mole of Concentration

Volume Mole of HCl
Samplin quenching HCl reacted NaOH of NaOH
of NaOH reacted with
g time HCl unreacted with NaOH unreacte unreacted
used NaOH in
(min) with NaOH in in sample d in with ethyl
(mL) sample
sample (mL) (mL) sample acetate (M)

0 21.6 8.64 1.36 0.000340 0.000340 0.00680

5 22 8.80 1.20 0.000300 0.000300 0.00600
10 24.3 9.72 0.28 0.000070 0.000070 0.00140
15 24.5 9.80 0.20 0.000050 0.000050 0.00100

Table 5. Data obtained for impeller speed at 4.5 rpm.

Volume of Volume of Concentration

Volume Mole of HCl Mole of
Sampling quenching HCl reacted of NaOH
of NaOH reacted with NaOH
time HCl unreacted with NaOH unreacted
used NaOH in unreacted
(min) with NaOH in in sample with ethyl
(mL) sample in sample
sample (mL) (mL) acetate (M)
0 23.3 9.32 0.68 0.000170 0.000170 0.00340
5 24.9 9.96 0.04 0.000010 0.000010 0.00020
10 25 10.00 0.00 0.000000 0.000000 0.00000
15 25 10.00 0.00 0.000000 0.000000 0.00000

Table 6. Data obtained for impeller speed at 6.5 rpm.

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 Concentration of NaOH unreacted with ethyl
acetate VS Time
0.012
Concentration of NaOH unreacted with
0.010

0.008
ethyl acetate (Mol/L)

0.006 1.5 rpm

0.004 4.5 rpm

6.5 rpm
0.002

0.000
0 5 10 15 20
Time (min)

Figure 4. Concentration of NaOH unreacted with ethyl acetate Vs Time

6
Discussion

Continuous Stirred Tank Reactor (CSTR) is a chemical reactor which is used very
commonly in the chemical industry. In both of the experiments, a batch CSTR is studied with
the same reactants concentration is 5 L of 0.05 M NaOH and 5 L of 0.05 M EtOAc. The
impeller speed is set constant at 4.5 rpm. Samples of 50 ml are taken at sampling time of 1
min, 5 min, 10 min and 15 min. Since this a batch process, reactants are not continuously
added and products are not continuously removed. The sample of reaction is collected and
added with 10 ml of 0.25 Mol/L hydrochloric acid (HCL) and 3 drops of indicator,
phenolphthalein for the titration process. The purpose of this to determine the unreacted
amount of sodium hydroxide in the sample. Titration is done until the solution turns pink.
The reaction that is used in this reaction is the hydrolysis of ethyl acetate with sodium
hydroxide to produce ethanol and sodium acetate. This is also called the saponification
reaction. The reaction equation is as NaOH + CH3COOC2H5 → CH3COONA + CH3CH2OH,
this is an irreversible reaction. Basically the ester, CH3COOC2H5 reacts with the base, NaOH
to produce a carboxylate salt, CH3COONA and alcohol CH3CH2OH. This is also an
endothermic reaction.

Three different graphs are plotted to identify the order of the reactions and then the
rate constants. Figure 1 shows the graph for first order reaction, Figure 2 for second order
reaction and Figure 3 for third order reaction. To measure the linearity of the graph plotted,
regression values is used, the higher the regression value the more linear the graph. The
regression value for this graphs are obtained by using the built in excel function. For Figure
1, the regression value is 0.9092 for the graph of ln (CA) versus time. For Figure 2, the
regression value is 0.932 for the graph of 1/CA versus time. For the figure 3, the regression
value is 0.8911 for the graph of 1/CA2 versus time. The highest regression value is from the
graph in Figure 2 which is 0.932, the most linear. Thus the reaction is second order reaction
based on this experiment, and is correct theoretically. The rate constant for second order
reactions are the gradient of the graph, it is also obtained from the straight line equation from
excel, y= 66.87x – 11.26. Thus the rate constant is 66.87 (Mol/L)-1min-1.

The second experiment was carried at different impeller speeds, and other methods
similar to the first experiment. Rate of reaction is the speed at which a chemical reaction
proceeds. Based on Figure 4, the trend is at higher impeller speed the lower the concentration
of NaOH unreacted with ethyl acetate (Mol/L) at their respective sampling time. When the

7
impeller speed increases the, the rate of mixing increases, causing high kinetic energy and
contact area for the reacting particles. The more the collision due to this, the higher the
chance for this reactants to be converted into products. It can also be noted that at impeller
speed of 6.5 rpm, at 5 minutes of sampling time the reaction is complete.

Conclusion

In conclusion, the order of the reaction is identified and the rate constant is also
identified. The saponification reaction between ethyl acetate, CH3COOC2H5 and sodium
hydroxide, NaOH is a second order reaction and has a rate constant of 66.87 (Mol/L)-1min-1.
The second experiment the speed was manipulated and the concentration of unreacted sodium
hydroxide (NaOH) is recorded. For the second experiment, it is found that when the impeller
speed of the CSTR increases, the rate of reaction increases, which is resembled by the lower
concentration of unreacted sodium hydroxide of the samples taken.

The might be some errors that have contributed to the results being slightly not
accurate. The first is human error, the titration process must be stopped the instance the
solution with the phenolphthalein changes colour. Thus the titration must be done drop by
drop slowly and carefully so that it is aware to us when suddenly the solution changes colour
to pink and to stop the titration. Next the contamination of the glassware used such as the
dropper, burette and the beaker. This beaker, burette and dropper must be cleaned with soap
to remove the contaminants so it will not affect the results obtained.

8
Reference

1) Data from K1 – Monday Session.

2) Çıtak, A., & Kıvrak, A. (2019). Determination of the Expression Rate of Ethyl Acetate
Hydrolysis Reaction Depending on the Temperature. Journal Of The Institute Of Science
And Technology, 382-388. doi: 10.21597/jist.410336

3) Borovinskaya R, Khaydarov V, Strehle N, (2019) Experimental Studies of Ethyl Acetate

Saponification. Retrieved from Applied Sciences MDPI

4) K. Al Mesfer (2017). Experimental Study of Batch Reactor Performance for Ethyl Acetate
Saponification. Retrieved from International Journal of Chemical Reactor Engineering,
Volume 16 , Issue 1.

Sample Calculations

1. Preparation of solution in the tank:

a) Volume of feed tank, VB1 = 5L
Initial concentration of NaOH, CNaOH = 0.05mol/L
Relative molecular mass of NaOH, MWNaOH = 40.0g/mol
No. of moles of NaOH = CNaOH x VB1
= 0.05 mol/L x 5L
= 0.25 mol
Mass of NaOH required = No. of moles of NaOH x RMMNaOH
= 0.25 mol x 40.0 g/mol
= 10 g
b) Volume of feed tank, VB2 = 5L
Initial concentration of ethyl acetate, CEtAc = 0.05 mol/L
Relative molecular mass of ethyl acetate, MWEtAc = 88.11g/mol
Purity of ethyl acetate = 100%
Density of ethyl acetate, ρ EtAc = 0.902 g/ml
100 0.902𝑔 𝑚𝑜𝑙 1000𝑚𝐿
Molarity of ethyl acetate=100 𝑥 𝑥 88.1𝑔 𝑥
𝑚𝑙 𝐿

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 =10.238mol/L
Volume of ethyl acetate,

𝑀1𝑉1 = 𝑀2𝑉2
10.238M 𝑥 𝑉1 =0.05 M 𝑥 5𝐿

𝑉1 = 0.0246L

𝑉EtAc = 24.6 𝑚𝑙

2. Preparation of solutions for titration:

a) NaOH
Concentration of NaOH required, CNaOH = 0.1mol/L
Relative molecular mass of NaOH, MWNaOH = 40.0g/mol
No. of moles of NaOH = CNaOH x Volume of solution

= 0.1 mol/L x 1 L
= 0.01 mol
Mass of NaOH required = Number of moles of NaOH x MWNaOH
= 0.01 mol x 40.0 g/mol
=4g

b) HCl
Concentration of HCl required, CHCl =0.25 mol/L
Purity of HCl = 100%
Density of HCl, ρ HCl = 1.3g/Ml
Relative molecular mass of HCl, MWHCl= 36.46g/mol
Volume of HCl required

= 0.25 M x 1 L x 36.46 g/mol x 1.3 g/mL

= 11.85 ml

3. Volume of each sample = 50 ml

Volume of quenching HCL unreacted with NaOH in sample, VHCL

unreacted

𝐶𝑁𝑎𝑂𝐻
VHCL unreacted = 𝑥 𝑉𝑁𝑎𝑂𝐻 𝑡𝑖𝑡𝑟𝑎𝑡𝑒𝑑
C𝐻𝐶𝑙

10
 0.1
= 𝑥 21.6𝑚𝑙
0.25
= 8.64 𝑚𝑙

Volume of HCL reacted with NaOH in sample, VHCL reacted

VHCL reacted = 𝑉𝐻𝐶𝐿 − 𝑉𝐻𝐶𝐿 𝑢𝑛𝑟𝑒𝑎𝑐𝑡𝑒𝑑

= (10 – 8.64)m𝑙

= 1.36 ml

Mole of HCl reacted with NaOH in sample = CHCl x VHCL reacted

= 0.25mol/L x (1.36/1000) L

= 0.000340mol

Mole of NaOH unreacted in sample = Mole of HCL reacted with NaOH in sample
= 0.000340 mol

Concentration of NaOH unreacted with EtAc, CNaOH unreacted

mole of NaOH unreacted in sample
CNaOH unreacted = 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒

0.001372 mol
= 50
𝐿
1000

= 0.00680 mol/L

Concentration of NaOH reacted with EtAc, CNaOH reacted

CNaOH reacted = 𝐶𝑁𝑎𝑂𝐻,initial − 𝐶𝑁𝑎𝑂𝐻,𝑢𝑛𝑟𝑒𝑎𝑐𝑡𝑒𝑑

= (0.05 − 0.00680)m𝑜𝑙/𝐿

= 0.0432 mol/L

Concentration of NaOH reacted

Conversion, X = 𝐼𝑛𝑖𝑡𝑖𝑎𝑙 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑖𝑛 𝑠𝑎𝑚𝑝𝑙𝑒

0.0432mol/L
= 0.05 mol/L

= 0.864

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