Group 1A - Lab Report Combine PDF

CDB 3052
CHEMICAL ENGINEERING LABORATORY (II)

SEPTEMBER 2019
Experiment : 2 – Plug Flow Tubular Reactor

Group : 1A
Group Members : Sherlyn Hee Yee Pei 25396
Phong Yue Jin 25197
Frederick Chong 17006349
Nuraienee Binti Jamingan 25248
Muhammad Ikmal Haziq bin Rahim 25357
Lab Instructor : Muhammad Qasim
Date : 11th October 2019
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Table of Contents
CHAPTER 1 INTRODUCTION & OBJECTIVES ....................................................................... 3
CHAPTER 2 METHODOLOGY ................................................................................................... 5
CHAPTER 3 RESULTS & DISCUSSION .................................................................................... 8
PART A: Preparation of the calibration curve for Conversion vs. Conductivity ..................................... 8
PART B: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide ................................ 9
ERRORS & RECOMMENDATIONS ................................................................................................... 15
CHAPTER 4 CONCLUSION....................................................................................................... 16
CHAPTER 5 REFERENCES ....................................................................................................... 17
CHAPTER 6 APPENDIX............................................................................................................. 18
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CHAPTER 1 INTRODUCTION & OBJECTIVES
INTRODUCTION
Plug flow reactor (PFR) is used for reactions in continuous, flowing system in a shape of
cylinder. PFR play a key role in chemical manufacturing facilities where a transformation of
chemical substances take place. In a plug flow reactor, feed is introduced from one end of a
cylindrical tube and flows continuously through the length of the reactor as a series of plugs (U.
P. L. Wijayarathne, 2014). The product is then collected from the other end of the reactor.
According to (Parimal, 2017), in an ideal plug flow reactor, specific assumptions are made
regarding the extent of mixing:
(1) No mixing in the axial direction

(2) Complete missing in the radial direction
(3) A uniform velocity profile across the radius
Plug Flow Reactor are usually used for a large-scale production, slow reactions, and
continuous reaction. Besides that, high temperature reaction usually done in the PFR. This is
because the PFR can withstand the high temperature of a reaction. PFR have a high volumetric
unit conversion and can run for a long period of time without maintenance (M. Danish, 2015).
That is why it is widely used in the manufacturing of chemicals.
For this experiment, the saponification reaction between sodium hydroxide and ethyl
acetate had been carried out using a plug flow tubular reactor (PFR) and the chemical equation is
as below:
NaOH + CH3COOC2H5 → CH3COONa + C2H3OH
This reaction can be assumed to be second order overall, first order in each reactant, with the
following rate expression:
Rate = k2CNaOHCEtOAc
Where k2= second order rate constant and CNaOH and CEtOAc are concentrations of NaOH and
EtOAc, respectively. The rate expression has the units [moles/(litre)(time)]. For these experiments,
the unit of time should be minutes.
3
In this experiment, a calibration curve which correlates the conductivity to the conversion
of the reactants is obtained. Then, the plug flow reactor was utilized to experiment on the effect of
residence time on the saponification process. Residence time is defined by a measure of how
much time the matter spends in the reactor. An ideal plug flow reactor has a fixed reactor time.
Any fluid that enters the reactor at time t0 will exit the reactor at time, t0 + τ, where τ is the residence
time of the reactor.
OBJECTIVES
This experiment involves the saponification reaction between ethyl acetate and sodium hydroxide
in a plug flow reactor. The objectives of this experiment are as follow:
1. To prepare the calibration curve for conversion versus conductivity

2. To determine the effects of residence time on the saponification of sodium hydroxide and
ethyl acetate.
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CHAPTER 2 METHODOLOGY
Apparatus: Plug flow tubular reactor
Material: Sodium Hydroxide, Ethyl Acetate, Water
Figure 1: The unit set up for plug flow reactor
Table 1: Labeling of the equipment for unit set up of a plug flow reactor
No. Equipment No. Equipment No. Equipment
1 Reactant tank 8 Reactor housing frame 15 Air regulator
2 Dosing pump 1 9 Overflow tube 16 Drain valve of reactant
tank 1 (V1)
3 Dosing pump 2 10 Level sensor 17 Drain valve of reactant
tank 1 (V2)
4 Reactor tubing coil 11 Heater 18 Drain valve of reactor
house tank (V3)
5 Conductivity Sensor 12 Solenoid valve 19 Drain valve of
production tank (V4)
6 Stirrer 13 Temperature control 20 Ball valve for air flowing
water bath circulator into inlet tubing 1 (V5)
7 Glass support cylinder 14 Waste tank 21 Ball valve for air flowing
into inlet tubing 2 (V6)
5
General Start-up Procedures
1. The following solutions is being prepared:

a. 15L of 0.1M sodium hydroxide, NaOH in reactant tank 1.
b. 15L of 0.1M ethyl acetate, Et(Ac) in reactant tank 2.
2. All valves are ensured to be initially closed.
3. The power for the control panel is turned on.
4. Valve V5 and V6 are opened and the air regulator is adjusted as small as possible to pump
the air into the tubing to clear the remained solutions inside the reactor tubing. Valve V5
and V6 are closed when there is no liquid inside the reactor tubing.
5. The plastic water hose is connected between water inlet solenoid valve and tap water that
is opened to half only.
6. The desired temperature for the following experiment is set on the Temperature Indicator
Control (TIC) panel.
7. The TIC switch is turned and the water filling button (green coloured button) is pushed to
fill up the water into the reactor until just below the overflow tube.
8. The stirrer is switched on to 100 RPM.
9. The computer is switched on and the corresponding software is clicked.
10. Pump P1 and P2 is switched on and both pumps are adjusted to obtain highest possible
flow rate into the reactor. The flow rate value is keyed in into the computer and run for
both pumps P1 (360 ml/min) and P2 (390 ml/min). The pump is switched off after the
chemicals coming into the reactor tubing coil.
General Shut-down Procedures
1. The temperature is set lower than that during the experiment on the TIC.
2. The cooling water is kept continuing flowing.
3. Pumps P1 and P2 is switched off. The stirrer is switched off.
4. The heater is switched off once the reactor cooled down to room temperature.
5. The power for control panel is turned off.
6. Valve V5 and V6 is opened.
7. Disposal valve V3 is opened to drain any liquid from reactor into waste tank.
6
8. The solutions are kept for subsequent experiment. Otherwise, valve V4 is opened to drain
all solutions from waste tank and valve V1 and V2 is opened to drain the remained
chemicals from the reactant tanks to barrels for storage respectively.
Experimental Procedures
Part A: Preparation of Calibration Curve for Conductivity vs Conversion
1. The calibration curve of conductivity vs conversion of saponification reaction of ethyl

acetate, Et(Ac) and sodium hydroxide, NaOH is retrieved online.
Part B: Saponification of Et(Ac) and NaOH in Plug Flow Reactor
1. The general start-up procedures are performed.

2. The temperature is set for 30 °C on the Temperature Indicator Control (TIC).
3. The flowrate of 50 ml/min is keyed into the computer and the flowrate is run for both
pumps P1 and P2. The flow rate of both pumps is recorded.
4. Pumps P1 and P2 is started at the same time. The timer is started immediately. In computer,
The Set Time Record is adjusted to 60s and “Start Record” button is clicked.
5. After 3 minutes, the outlet conductivity value is monitored until it does not change over
time to ensure reactor reached steady state.
6. The outlet conductivity value is recorded.
7. The concentration of NaOH exiting the reactor and extent of conversion is calculated from
the calibration curve.
8. Experiment is repeated from step 2 to 7 for different residence times. The feed flow rates
of NaOH and Et(Ac) is increased to 100, 150, 200, 250 and 300 ml/min.
9. The general shut-down procedures are performed.
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CHAPTER 3 RESULTS & DISCUSSION
PART A: Preparation of the calibration curve for Conversion vs. Conductivity
Coductivity Vs Conversion
12
10
Conductivity (mS/cm)
4
y = -0.0616x + 9.74
R² = 0.9747
2
0
0 20 40 60 80 100
Conversion, X (%)
Figure 2: Graph of Conductivity vs Conversion

The main objective of the experiment is to study the saponification of ethyl acetate and sodium
hydroxide. The chemical equation for saponification reaction is as below:
CH3COOCH2CH3 + NaOH → CH3COONa + CH3CH2OH

Ethyl Acetate Sodium Hydroxide Sodium Acetate Ethanol
Sodium hydroxide will act as limiting reactant and this reaction will produce sodium acetate.
In experiment Part A, a calibration curve for conversion vs conductivity as shown in Figure 2
above is plotted to determine the conversion value of the saponification of ethyl acetate and sodium
hydroxide to form sodium acetate in a plug flow reactor. The calibration curve of conductivity vs
conversion is plotted based on the experiment data retrieved from an online lab report entitled
“CHE244 - Lab Report Effect of Residence Time on The Reaction in TFR (2015).” Based on the
graph, it shows that when the conversion percentage increases the conductivity of the solution
decreases. This can be explained that the number of moles of hydroxide ion in the solution
deceases from 0 to 100% conversion. In another words, the number of ions per unit volume that
carry current in a solution decrease. Thus, conductivity is inversely proportional to the conversion.
The graph of conductivity vs conversion shows a linear trend. However, the linear trend is then
linearized to get a more accurate reading. This calibration graph has a negative gradient of -0.0616
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and y-intercept value of 9.74. This calibration curve exhibits a strong linear relationship and can
be used as reference purpose since the R2 value is 0.9747 which is close to unity.
PART B: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide
For this experiment, equimolar concentrations of reactants are used to avoid the system from
forming an exponential decay after long periods of time.
According to Kuheli Das (2011), the saponification reaction between ethyl acetate and sodium
hydroxide which is a strong base is an overall second order reaction with both reactants at first
order. Therefore, the rate law is represented by:
Given, the concentration of ethyl acetate, CA and sodium hydroxide, CB are the same at 0.1M for
this experiment.
−𝒓𝑨 = 𝒌𝑪𝑨 𝑪𝑩 = 𝒌𝑪𝟐𝑨
−𝒓𝑨 = 𝒌𝑪𝟐𝑨𝟎 (𝟏 − 𝑿)𝟐
Determination of reaction rate constant in terms of residence time
Residence time:
𝑽
𝝉=
𝒗𝟎
For PFR,
𝑿 𝑿
𝒅𝑿 𝒅𝑿
𝑽𝒐𝒍𝒖𝒎𝒆 = 𝑭𝑨𝟎 ∫ = 𝒗𝟎 𝑪𝑨𝟎 ∫ 𝟐 𝟐
𝟎 −𝒓𝑨 𝟎 𝒌𝑪𝑨𝟎 (𝟏 − 𝑿)
𝑿
𝒗𝟎 𝒅𝑿
𝑽= ∫
𝒌𝑪𝑨𝟎 𝟎 (𝟏 − 𝑿)𝟐
𝒗𝟎 𝑿
𝑽= ( )
𝒌𝑪𝑨𝟎 𝟏 − 𝑿
𝑽 𝟏 𝑿
𝝉= = ( )
𝒗𝟎 𝒌𝑪𝑨𝟎 𝟏 − 𝑿
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𝒗𝟎 𝑿
𝑹𝒆𝒂𝒄𝒕𝒊𝒐𝒏 𝒓𝒂𝒕𝒆 𝒄𝒐𝒏𝒔𝒕𝒂𝒏𝒕, 𝒌 = ( )
𝑽𝑪𝑨𝟎 𝟏 − 𝑿
for PFR with constant volume, initial feed flowrate and reactants’ concentrations.
Table 2: The data of volumetric flowrate, conductivity and values of residence time, conversion,
reaction rate constant as well as rate of reaction
NaOH Et (Ac) Total Residenc Average Conver Fraction Reaction Rate

flowrate flowrate feed e time, outlet sion, X of rate of
(mL/min) (mL/min) flowrate, (min) conductivity (%) conversio constant reaction, -
v0 (mS/cm) n, X , rA (mol/L
(mL/min) k (L/mol min)
min)
300 300 600 0.658 6.851 46.90 0.469 13.423 0.0378
250 250 500 0.790 6.812 47.53 0.475 11.473 0.0316
200 200 400 0.987 6.561 51.61 0.516 10.805 0.0253
150 150 300 1.316 6.551 51.77 0.518 8.156 0.0190
100 100 200 1.974 5.873 62.78 0.628 8.543 0.0118
50 50 100 3.948 6.562 51.59 0.516 2.699 0.0063
Residence Time vs. Total Feed Flowrate

4.5
4
Residence time, (min)
3.5
3
2.5
2
1.5
1
0.5
0
0 100 200 300 400 500 600 700
Total feed flowrate, v0 (mL/min)
Figure 3: Graph of Residence Time vs. Total Feed Flowrate
Residence time, is also known as space time which is the period necessary to process one reactor
volume of fluid at entrance conditions. It is denoted by the formula:
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𝐕𝐫𝐞𝐚𝐜𝐭𝐨𝐫 𝐕𝐨𝐥𝐮𝐦𝐞 𝐨𝐟 𝐫𝐞𝐚𝐜𝐭𝐨𝐫
𝛕= =
𝐯𝟎 𝐕𝐨𝐥𝐮𝐦𝐞𝐭𝐫𝐢𝐜 𝐟𝐥𝐨𝐰𝐫𝐚𝐭𝐞
Figure 3 shows that the residence time decreases with the increase in total inlet flowrate. This is
because at higher inlet reactants’ flowrates, the solution flows faster through the reactor. Hence,
the time the reactants stay in the reactor is shorter leading to a shorter residence time.
Average Outlet Conductivity vs. Residence Time

7
Average outlet conductivity (mS/cm)
6.8
6.6
6.4
6.2
6 y = -0.095x + 6.6881
5.8
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
Figure 4 Graph of Average Outlet Conductivity vs. Residence Time

The graph in Figure 4 indicates a negative slope which means that the outlet conductivity of the
solution decreases with higher residence time. This is shown by the outlet conductivity which is
maximum at 6.851 mS/cm during the lowest residence time of 0.658 min. Since the lowest
residence time corresponds to the highest inlet volumetric flowrate, hence, the reactants’ solution
is at the maximum inlet flowrate of 600 mL/min. Therefore, the conductivity of the solution
increases with the inlet solution’s flowrate. This is because the conductivity of the solution is
affected by the concentration of ions in the water which are released during the dissociation of
NaOH in water into sodium and hydroxide ions. Ethyl acetate solution does not affect the
conductivity because it is an alcohol. Moreover, conductivity is the ability of the solution to carry
electric current through the solution by the presence of ions. Therefore, at higher flowrates of
reactants which includes NaOH solution, the higher the concentration of ions in the solution, the
better its’ conductivity. Based on Figure 4, the conductivity steadily drops with it reaches the
minimum point at residence time of 5.873 mS/cm at 100 mL/min. Since, based on Figure 2, the
conductivity and conversion are inversely proportional. Thus, this condition relates to the
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maximum conversion. This is because the maximum conversion of ethyl acetate is achieved during
that point of time. Thus, based on Figure 2, the conductivity and conversion are inversely
proportional, so the conductivity drops to the minimum value before increasing again due to the
drop-in conversion. The fluctuations in values could also be due to error conducted during the
experiment which will be further discussed in the Errors & Recommendations section.
Conversion vs. Residence Time

70.00
65.00
y = 1.5418x + 49.544
Conversion, X (%)
60.00
55.00
50.00
45.00
40.00
0 1 2 3 4 5
Figure 5: Graph of Conversion of Ethyl Acetate vs. Residence Time

Figure 5 shows that the conversion of ethyl acetate rises with residence time from the positive
slope value. The conversion increases from 46.90 % to 62.78 % for the residence time from 0.658
min to 1.974 min. Since residence time is inversely proportional to the inlet volumetric flowrate,
the reaction conversion drops with lower feed volumetric flowrates. This is because with higher
feed flowrates, the time the reactants spend in the reactor is shorter leading to lower product
formation which is shown by the lower conversion value. Therefore, for practical applications,
higher reactants flowrates are not always considered desirable (AboGhander, 2006). Theoretically,
the conversion versus residence time depicts a linear relationship. However, after reaching the
desired conversion which is the maximum it becomes constant with time (Danish, 2015) due to
the decrease in concentration of limiting reactant. This is shown by the decrease in conversion
from 62.78% to 51.59% after residence time of 1.974 min. This is also affected by the random and
systematic errors posed during the experiment. Most importantly, the presence of air bubbles in
the pfr tubes could lead to fluctuations in the conductivity readings and the poor condition of the
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conductivity sensor due to rusting or long periods of usage could lead to lower sensitivity in taking
readings.
Reaction Rate Constant vs. Total Feed Flowrate

16
Reaction rate constant, k (L/mol min)
14 y = 0.0186x + 2.6778
12
10
8
6
4
2
0
0 100 200 300 400 500 600 700
Figure 6 Graph of Reaction Rate Constant of saponification reaction of Sodium Hydroxide and
Ethyl Acetate vs. Total Feed Flowrate
The reaction rate constant increases with total feed flowrate as shown in Figure 6. This is due to
their directly proportional relation in the formula:
𝒗𝟎 𝑿
𝒌= ( )
for PFR with constant volume, initial feed flowrate and reactants’ concentrations.
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Rate of Reaction vs. Total Feed Flowrate
0.0400
Rate of reaction, -rA (mol/L min)

0.0350 y = 6E-05x - 0.0003
0.0300
0.0250
0.0200
0.0150
0.0100
0.0050
0.0000
0 100 200 300 400 500 600 700
Figure 7 Graph of Rate of Reaction of saponification reaction of Sodium Hydroxide and Ethyl
Acetate vs. Total Feed Flowrate
Figure 7 shows a linear relation between the rate of reaction and feed flowrate. Since the
saponification reaction of ethyl acetate and sodium hydroxide is a second order reaction, the rate
law can be represented by:
−𝒓𝑨 = 𝒌𝑪𝟐𝑨𝟎 (𝟏 − 𝑿)𝟐
Thus, based on the rate law, when the feed flowrate increases, the conversion of ethyl acetate
decreases and reaction rate constant rises leading to a higher rate of reaction. The rate of reaction
is also defined as the change in concentration of reactants over time. For a constant time period,
the lower the change in reactants (lower conversion) due to higher feed flowrates leads to higher
reaction rates.
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ERRORS & RECOMMENDATIONS
Systematic Error
In this experiment, the formation of air bubbles within the tube causes a disturbance in the
reading of conductivity. When there are air bubbles, it disrupts the system by preventing radial
mixing of the fluids, which is very crucial in the reaction of the reactor. The presence of air bubbles
also results in the decrease in the volume of PFR because it is filled with air rather than the reactants
and this reduction in effective volume results in error in the data collected. To overcome this error,
the absence of air bubbles in the system must be ensured by using suitable flowrate and allow the
system to run until most or all of the air bubbles are excreted.
Besides that, there may also be contamination of NaOH and Et (Ac) in the tanks as there
were residues left in the tanks before the experiment started. These residues may consist
contaminant which will affect the reaction by affecting the concentration of the solutions prepared
thus affecting also the conductivity obtained. Hence, it is recommended to discard the residual
chemicals that are left in the tank and rinse the tan before pouring the fresh chemical prepared into
the tank.
Random Error
During the experiment, two solutions were prepared, which are sodium hydroxide and ethyl
acetate. Human error could occur during the preparation of the mixture when the eyes are not
perpendicular to the reading scale. This may be corrected by ensuring the eye level is always
perpendicular to the reading scale during the preparation of sample. Moreover, the weighing of
solid reactant may be inaccurate as there may be slightly excess or lacking reactant. This may be
overcome by pre-determining correctly the weight of solid before conducting the experiment.
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CHAPTER 4 CONCLUSION
In this experiment, the saponification reaction between sodium hydroxide (NaOH) and
ethyl acetate (Et(Ac)) in a plug flow reactor (PFR) is studied. The inlet flow rate is varied to
observe the effect on residence time, conversion and ultimately, reaction rate. The outlet
conductivity is measured and can be corelated to conversion using a calibration curve. The
calibration curve is a linearized equation which determines the conductivity value at varying
conversion of NaOH. The residence time is the ratio of volume of reactor to the total inlet flow
rate. Thus, it decreases with increasing flow rate. Furthermore, conversion is found to increase
when residence time increases. Theoretically, this is the case as the formation of products can
occur for a longer time as the reactants spent more time flowing through the reactor. Reaction rate
constant is then calculated from the mole balance equation and is found to depict an increasing
pattern with increasing inlet flow rate. The rate of reaction of second order is higher with higher
rate constant and lower conversion whereby it reaches 0.0378 mol/L min when total inlet flow rate
is maximum. At maximum total inlet flow rate, residence time is minimum which gives lowest
conversion and rate constant is also observed to peaked at that point. These correlations result in
rate of reaction to be the highest.
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CHAPTER 5 REFERENCES
Hye Ji Lee, D. H. (2018). Transition Phase Approach for Statistical Model in Multiphase
Process. Seoul: Elsevier.
Kuheli Das, S. B. (2011). Kinetic Studies on Saponification of Ethyl Acetate Using an
Innovative Conductivity-Monitoring Instrument with a Pulsating Sensor. International
Journal of Chemical Kinetics, 648-656.
M. Danish, A. M. (2015). A Comparative Study of Saponification Reaction in a PFR and CSTR.
Research Journal of Chemical Sciences , 13-17.
Mohd Danish, M. K. (2015). Effect of Operating Conditions on CSTR performance: an
Experimental Study. International Journal of Engineering Research and Applications,
74-78.
Nabeel S. AboGhander, A. A. (2006). A Chemical Reaction Engineering Laboratory
Experiment: Isothermal Laminar-Flow Reactor. Engineering Education.
Parimal. (2017). Biological Treatment Technology. Industrial Water Treatment Process
Technology, 65-144.
Pranay, K. (2016, March 4). Quora. Retrieved from Does conversion depend on residence time
or space time?: https://www.quora.com/Does-conversion-depend-on-residence-time-or-
space-time
Syahiirah, N. (2018). academia. Retrieved from CHE506 - Lab Report On Plug Flow Reactor:
https://www.academia.edu/37932046/CHE506_-
_Lab_Report_On_Plug_Flow_Reactor_L5_2018_
U. P. L. Wijayarathne, K. C. (2014). Aspen Plus Simulation of Saponification of Ethyl Acetate in
the Presence of Sodium Hydroxide in a Plug Flow Reactor . International Journal of
Chemical and Molecular Engineering, 1089-1096.
UMich. (2019, October 2). Retrieved from
http://umich.edu/~elements/5e/asyLearn/bits/batch/index.htm
17
CHAPTER 6 APPENDIX
Part A: Preparation of the calibration curve for Conversion vs. Conductivity
Table 3: Data for Preparation of Calibration Curve
Conversion Solution Mixture (ml) Concentration Conductivity

(%) 0.1 M NaOH 0.1 M Na H2O of NaOH (M) (mS/cm)
(Ac)
0 100 0 100 0.0500 10.2
25 75 25 100 0.0375 7.9
50 50 50 100 0.0250 6.2
75 25 75 100 0.0125 5.1
100 0 100 100 0.0000 3.9
Calculation
1. Calculate the mass of Sodium Hydroxide, NaOH for 1L of 0.025M NaOH
MW of NaOH = 40 g/mol
Mass of NaOH = (0.025M)(40g/mol)(1L) = 1g NaOH
∴ To make 0.025M NaOH solution, dilute 1g of NaOH in 1L water
2. Calculate the mass of Sodium Acetate, CH3COONa for 1L of 0.025M CH3COONa

MW of CH3COONa = 136.08 g/mol
Mass of CH3COONa = (0.025M)(136.08g/mol)(1L) = 3.402g CH3COONa
∴ To make 0.025M CH3COONa solution, dilute 2.05g of CH3COONa in 1L water
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Part B: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide
Calculation of the volume of the plug flow reactor

V = πr2 × 2πR(N)
The size of the tubes = 6 x 4 mm
Radius of tubes (r) = 2 mm
Number of coils (N) = 60
Radius of coils (R) = 100 mm
Length of tube (L) = 2πr = 2π(0.1 m) = 0.628 m
Volume of PFR = π(0.002 m)2 × 0.628 m (50) = 3.948 × 10-4 m3 = 0.3948 L = 394.8 mL
Calculation of the residence time
The residence time can be calculated using the following equation:
𝐕𝐫𝐞𝐚𝐜𝐭𝐨𝐫 𝐕𝐨𝐥𝐮𝐦𝐞 𝐨𝐟 𝐫𝐞𝐚𝐜𝐭𝐨𝐫

𝛕= =
𝐯𝟎 𝐕𝐨𝐥𝐮𝐦𝐞𝐭𝐫𝐢𝐜 𝐟𝐥𝐨𝐰𝐫𝐚𝐭𝐞
Vreactor = 394.8 mL
𝐕𝐫𝐞𝐚𝐜𝐭𝐨𝐫 𝟑𝟗𝟒.𝟖 𝐦𝐋
For vo= 100 mL/min, 𝛕 = = 𝟏𝟎𝟎 𝐦𝐋/𝐦𝐢𝐧 = 𝟑. 𝟗𝟒𝟖 𝒎𝒊𝒏
𝐯𝟎
For vo= 200 mL/min, 𝛕 = = 𝟐𝟎𝟎 𝐦𝐋/𝐦𝐢𝐧 = 𝟏. 𝟗𝟕𝟒 𝒎𝒊𝒏
𝐯𝟎
For vo= 300 mL/min, 𝛕 = = 𝟑𝟎𝟎 𝐦𝐋/𝐦𝐢𝐧 = 𝟏. 𝟑𝟏𝟔 𝒎𝒊𝒏
𝐯𝟎
For vo= 400 mL/min, 𝛕 = = 𝟒𝟎𝟎 𝐦𝐋/𝐦𝐢𝐧 = 𝟎. 𝟗𝟖𝟕 𝒎𝒊𝒏
𝐯𝟎
For vo= 500 mL/min, 𝛕 = = 𝟓𝟎𝟎 𝐦𝐋/𝐦𝐢𝐧 = 𝟎. 𝟕𝟖𝟗𝟔 𝒎𝒊𝒏
𝐯𝟎
For vo= 600 mL/min, 𝛕 = = 𝟔𝟎𝟎 𝐦𝐋/𝐦𝐢𝐧 = 𝟎. 𝟔𝟓𝟖 𝒎𝒊𝒏
𝐯𝟎
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Calculation of conversion
The value of conversion can be calculated using the equation from the calibration curve, where
the equation of the graph is given as below:
y = -0.0616x + 9.74
where
y = conductivity
x = conversion
After rearranging, the equation to find the conversion is as below:
𝒚 − 𝟗. 𝟕𝟒
𝒙=
−𝟎. 𝟎𝟔𝟏𝟔
For v0 = 0.1 L/min and average outlet conductivity, y = 6.562 mS/cm,
𝟔. 𝟓𝟔𝟐 − 𝟗. 𝟕𝟒
𝒙= = 𝟓𝟏. 𝟓𝟗 %
−𝟎. 𝟎𝟔𝟏𝟔
𝟓. 𝟖𝟕𝟑 − 𝟗. 𝟕𝟒
𝒙= = 𝟔𝟐. 𝟕𝟖 %
−𝟎. 𝟎𝟔𝟏𝟔
𝟔. 𝟓𝟓𝟏 − 𝟗. 𝟕𝟒
𝒙= = 𝟓𝟏. 𝟕𝟕 %
−𝟎. 𝟎𝟔𝟏𝟔
𝟔. 𝟓𝟔𝟏 − 𝟗. 𝟕𝟒
𝒙= = 𝟓𝟏. 𝟔𝟏 %
−𝟎. 𝟎𝟔𝟏𝟔
𝟔. 𝟖𝟏𝟐 − 𝟗. 𝟕𝟒
𝒙= = 𝟒𝟕. 𝟓𝟑 %
−𝟎. 𝟎𝟔𝟏𝟔
20
𝟔. 𝟖𝟓𝟏 − 𝟗. 𝟕𝟒
𝒙= = 𝟒𝟔. 𝟗𝟎 %
−𝟎. 𝟎𝟔𝟏𝟔
Calculation of the rate constant, k (L/mol.min)
The rate constant can be calculated from the following equation:
𝒗𝟎 𝑿
𝒌= ( )
𝑳
𝒗 𝑿 𝟎.𝟔 𝟎.𝟒𝟔𝟗 𝑳
For vo= 0.6 L/min, 𝒌 = 𝑽𝑪𝟎 (𝟏−𝑿) = 𝒎𝒊𝒏
𝒎𝒐𝒍 (𝟏−𝟎.𝟒𝟔𝟗) = 𝟏𝟑. 𝟒𝟐𝟑 𝒎𝒐𝒍.𝒎𝒊𝒏
𝑨𝟎 𝟎.𝟑𝟗𝟒𝟖 𝑳 (𝟎.𝟏 )
𝑳
𝑳
𝒗𝟎 𝑿 𝟎.𝟓 𝟎.𝟒𝟕𝟓 𝑳
For vo= 0.5 L/min, 𝒌 = 𝑽𝑪 (𝟏−𝑿) = 𝒎𝒊𝒏
𝒎𝒐𝒍 (𝟏−𝟎.𝟒𝟕𝟓) = 𝟏𝟏. 𝟒𝟕𝟑 𝒎𝒐𝒍.𝒎𝒊𝒏
𝑨𝟎 𝟎.𝟑𝟗𝟒𝟖 𝑳 (𝟎.𝟏 )
𝑳
𝑳
𝒗 𝑿 𝟎.𝟒 𝟎.𝟓𝟏𝟔 𝑳
𝒎𝒐𝒍 (𝟏−𝟎.𝟓𝟏𝟔) = 𝟏𝟎. 𝟖𝟎𝟓 𝒎𝒐𝒍.𝒎𝒊𝒏
𝑨𝟎 𝟎.𝟑𝟗𝟒𝟖 𝑳 (𝟎.𝟏 )
𝑳
𝑳
𝒗 𝑿 𝟎.𝟑 𝟎.𝟓𝟏𝟖 𝑳
𝒎𝒐𝒍 (𝟏−𝟎.𝟓𝟏𝟖) = 𝟖. 𝟏𝟓𝟔 𝒎𝒐𝒍.𝒎𝒊𝒏
𝑨𝟎 𝟎.𝟑𝟗𝟒𝟖 𝑳 (𝟎.𝟏 )
𝑳
𝑳
𝒗𝟎 𝑿 𝟎.𝟐 𝟎.𝟔𝟐𝟖 𝑳
For vo= 0.2 L/min, 𝒌 = 𝑽𝑪 (𝟏−𝑿) = 𝒎𝒊𝒏
𝒎𝒐𝒍 (𝟏−𝟎.𝟔𝟐𝟖) = 𝟖. 𝟓𝟒𝟑 𝒎𝒐𝒍.𝒎𝒊𝒏
𝑨𝟎 𝟎.𝟑𝟗𝟒𝟖 𝑳 (𝟎.𝟏 )
𝑳
𝑳
𝒗 𝑿 𝟎.𝟏 𝟎.𝟓𝟏𝟔 𝑳
𝒎𝒐𝒍 (𝟏−𝟎.𝟓𝟏𝟔) = 𝟐. 𝟔𝟗𝟗 𝒎𝒐𝒍.𝒎𝒊𝒏
𝑨𝟎 𝟎.𝟑𝟗𝟒𝟖 𝑳 (𝟎.𝟏 )
𝑳
21
Calculation of reaction rate, -rA (mol/L.min)
The reaction rate can be calculated using the following equation:

-rA= kCA0CB0(1-X)2
Second order reaction, CA0 = CB0 = 0.1 M,
-rA= kCA02(1-X)2
𝑳 𝒎𝒐𝒍 𝟐 𝒎𝒐𝒍
For v0= 0.1 L/min, −𝒓𝑨 = 𝟐. 𝟔𝟗𝟗 𝒎𝒐𝒍.𝒎𝒊𝒏 (𝟎. 𝟏 ) (𝟏 − 𝟎. 𝟓𝟏𝟔)𝟐 = 𝟎. 𝟎𝟎𝟔𝟑 𝑳.𝒎𝒊𝒏
𝑳
For v0= 0.2 L/min,
−𝒓𝑨 = 𝟖. 𝟓𝟒𝟑 (𝟎. 𝟏 ) (𝟏 − 𝟎. 𝟔𝟐𝟖)𝟐 = 𝟎. 𝟎𝟏𝟏𝟖
𝒎𝒐𝒍. 𝒎𝒊𝒏 𝑳 𝑳. 𝒎𝒊𝒏
For v0= 0.3 L/min,
−𝒓𝑨 = 𝟖. 𝟏𝟓𝟔 (𝟎. 𝟏 ) (𝟏 − 𝟎. 𝟓𝟏𝟖)𝟐 = 𝟎. 𝟎𝟏𝟗𝟎
𝒎𝒐𝒍. 𝒎𝒊𝒏 𝑳 𝑳. 𝒎𝒊𝒏
For v0= 0.4 L/min, −𝒓𝑨 = 𝟏𝟎. 𝟖𝟎𝟓 𝒎𝒐𝒍.𝒎𝒊𝒏 (𝟎. 𝟏 ) (𝟏 − 𝟎. 𝟓𝟏𝟔)𝟐 = 𝟎. 𝟎𝟐𝟓𝟑 𝑳.𝒎𝒊𝒏
𝑳
For v0= 0.5 L/min, −𝒓𝑨 = 𝟏𝟏. 𝟒𝟕𝟑 𝒎𝒐𝒍.𝒎𝒊𝒏 (𝟎. 𝟏 ) (𝟏 − 𝟎. 𝟒𝟕𝟓)𝟐 = 𝟎. 𝟎𝟑𝟏𝟔 𝑳.𝒎𝒊𝒏
𝑳
For v0= 0.1 L/min, −𝒓𝑨 = 𝟏𝟑. 𝟒𝟐𝟑 𝒎𝒐𝒍.𝒎𝒊𝒏 (𝟎. 𝟏 ) (𝟏 − 𝟎. 𝟒𝟔𝟗)𝟐 = 𝟎. 𝟎𝟑𝟕𝟖 𝑳.𝒎𝒊𝒏
𝑳
22
23
CDB 3052
SEPTEMBER 2019
Experiment : 4 – Batch Liquid Reactor

Group : 1A
Phong Yue Jin 25197
Lab Instructor : Masooma Nazar
Date : 4th October 2019
1
TABLE OF CONTENTS
CHAPTER 1 INTRODUCTION & OBJECTIVES .................................................................. 3
CHAPTER 2 METHODOLODY……………………………………………………………..4-5
CHAPTER 3 RESULTS & DISCUSSION ................................................................................. 6
PART A: Preparation of the calibration curve for Conversion vs. Conductivity ........... 6-7
PART B: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide ..... 7-12
ERRORS & RECOMMENDATION ............................................................................... 12-13
CHAPTER 4 CONCLUSION .................................................................................................... 14
CHAPTER 5 REFERENCES .................................................................................................... 15
CHAPTER 6 APPENDIX ..................................................................................................... 16-20
2
INTRODUCTION
Batch reactors are usually used when a company wants to produce a range of products
involving different reactants and reactor conditions. They can then use the same equipment for
these reactions. Example of some processes that produce small quantities of high-valued materials
using batch reactors are cell cultivation, polymer synthesis and crystallization (Hye Ji Lee,
2018). Batch reactors are charged via two holes in the top of the tank. While the reaction is carried
out, nothing else is put in or taken out until the reaction is done. The reactor tank can be easily
heated or cooled by the jacket (UMich, 2019). Some advantages of using a batch reactor include
high conversion per unit volume, flexibility of operation and easy to clean. There is no feed and
exit streams in a batch reactor. Thus, the equation of batch liquid reactor is shown as below:
The rate of reaction of component A is defined as:
By this definition, if A is a reaction product, the rate is positive; whereas if it is a reactant which
is consumed, the rate is negative. Hence the equation is simplified to:
OBJECTIVES
This experiment involves the saponification reaction between ethyl acetate and sodium hydroxide
in a batch reactor. The objectives of this experiment are as follow:
1. To prepare the calibration curve for conversion versus conductivity
2. To study the batch saponification reaction of Ethyl Acetate and Sodium Hydroxide
3
CHAPTER 2 METHODOLOGY
Apparatus: Reactor, Feed Inlet System, Water Bath, Product/Waste Tank, Control Panel, Data
Acquisition System
Material: Sodium Hydroxide, Ethyl Acetate, Water
Figure 1: The unit set up for batch reactor
Experimental Procedure
1) The following solutions are prepared based on the table below by mixing NaOH solution
with Sodium Acetate and water.
Table 1: Preparation of different conversion solution for calibration
Conversion Solution
0.00 1-L of 0.05M NaOH
0.25 1-L of 0.075M NaOH + 1-L of 0.025M Sodium Acetate
1.00 1-L of 0.05M Sodium Acetate
4
2) The tap water is used to rinse the batch reactor before beginning the experiment.
3) SOLDAS Data Acquisition System is turned on.
4) First, 1-L of 0.05M NaOH (0 conversion) is poured into the batch liquid reactor using a
filter funnel.
5) The power of the batch reactor is switched on.
6) The RPM of the stirrer is fixed at 200rpm for 12 minutes.
7) The data is recorded for every interval of 60 seconds until 12 data is recorded.
8) The batch reactor is cleaned with tap water and the data is reset.
9) The experiment is repeated with different conversion solution (0.25, 0.50, 0.75, 1)
respectively.
10) The graph of conversion vs conductivity is plotted.
11) The slope and y-axis intercept from the plot of conversion vs. conductivity are analysed.

1) The batch reactor is cleaned with tap water.
2) The data in SOLIDAS Data Acquisition System is reset.
3) The batch reactor is cleaned with tap water.
4) 1-L of 0.1 M Ethyl Acetate and 1 M NaOH are poured into the batch reactor using a filter
funnel.
5) The power of the batch reactor is switched on.
6) The RPM of the stirrer is set to 50RPM for 12 minutes.
7) The data is recorded for every interval of 60 seconds until 12 data is recorded.
8) The experiment is repeated by changing the stirrer RPM to 100, 150 and 200 respectively
while using the same solution.
9) The batch reactor is cleaned with tap water and the data is reset.
10) The graph of order of reaction is plotted and the rate constant is determined from the graph.
5
Calibration Curve: Conversion vs Conductivity

1.00
0.90
0.80
0.70
Conversion
0.60
0.50
0.40
0.30 y = -0.1094x + 2.0139
R² = 0.9974
0.20
0.10
0.00
8.00 10.00 12.00 14.00 16.00 18.00 20.00
Figure 2: Calibration curve graph for conversion vs conductivity.

The main objective of the experiment is to study the saponification of ethyl acetate and sodium
hydroxide. The chemical equation for saponification reaction is as below.
CH3COOCH2CH3 + NaOH → CH3COONa + CH3CH2OH

Ethyl Acetate Sodium Hydroxide Sodium Acetate Ethanol
Sodium hydroxide will act as limiting reactant and this reaction will produce sodium acetate.
Throughout the experiment, the conductivity of the solution in the batch reactor will be recorded.
The conversion of the reaction corresponding to the conductivity can be calculated using the linear
equation of the calibration curve. Hence, simulations with different concentrations of sodium
hydroxide and sodium acetate was carried out to obtain the calibration curve.
In experiment Part A, a calibration curve for conversion vs conductivity as shown in Figure 2

above is plotted to determine the conversion value of the saponification of ethyl acetate and sodium
hydroxide to form sodium acetate in a batch reactor for experiment Part B. Sodium hydroxide have
larger molar conductivity than sodium acetate. This can be seen in the Figure 2 where at maximum
conversion, sodium acetate has the least conductivity while at zero-conversion sodium hydroxide
6
has the largest conductivity in the solution. The calibration curve shows that the conversion is
inversely proportional to the conductivity of the solution. This is because sodium hydroxide is a
strong base electrolyte consist of high concentration of freely moving hydroxide ions, OH- while
sodium acetate is a weak electrolyte consist of acetate ions, CH3COO-. As the sodium acetate
forms, the conductivity of the solution decreases as sodium acetate is a weaker base. The study
obtained is proven by the experiment as the conductivity of the solution decrease as the conversion
increased. From the calibration curve in Figure 2, we can calculate the conversion of ethyl acetate
and sodium hydroxide reaction for every different RPM. The trendline equation: y = -
0.1094x+2.0139 where y = conversion and x = conductivity can be used to find the conversion by
substituting the corresponding conductivity value into the equation.
Conductivity vs Time
20
18
16
50 RPM
14
100 RPM
12 150 RPM
10 200 RPM
50 RPM : y = -0.246x + 16.998 150 RPM : y = -0.004x + 14.078 Linear (50 RPM)
8 R² = 0.2426
R² = 0.8928
Linear (50 RPM)
6
100 RPM : y = -0.0287x + 14.38 200 RPM : y = 0.0003x + 14.015 Linear (100 RPM)
4
R² = 0.9646 R² = 0.0025 Linear (150 RPM)
2
Linear (200 RPM)
0
1 2 3 4 5 6 7 8 9 10 11 12
Time (min)
Figure 3: Graph for Conductivity vs Time
7
Conversion vs Time 50 RPM
100 RPM
0.6
150 RPM
0.5 200 RPM

Linear (50 RPM)
0.4 Linear (100 RPM)

Conversion
Linear (150 RPM)

0.3 Linear (200 RPM)
0.2 50 RPM: y = 0.0269x + 0.1543

R² = 0.8928
0.1 100 RPM : y = 0.0031x + 0.4408
R² = 0.9642
0 150 RPM: y = 0.0004x + 0.4738

0 2 4 6 8 10 12 14 R² = 0.2409
Time (min) 200 RPM: y = -3E-05x + 0.4806
R² = 0.0025
Figure 4: Graph for Conversion vs Time

This experiment was conducted by varying the rotational speeds of the stirrer by 200, 150,
100 and 50 RPM. 1 L of 0.1 M sodium hydroxide solution and 1 L of 0.1 M ethyl acetate solution
was added into the batch reactor. The conductivity of the mixture is observed every 60 seconds.
The main objective of this experiment is to study the saponification of ethyl acetate and sodium
hydroxide. Conductivity of a substance represents the number of ions present in that substance.
For this experiment, conductivity of the solution is due to the presence of hydroxide ion (OH-)
from sodium hydroxide. From the graph of Conductivity vs Time in Figure 3, for 50 RPM, the
conductivity of the solution decreases as the time increase. In Figure 4, the conversion increase as
the time increase for 50 RPM. This show that as the time passes, more ions reacted, which cause
the presence OH- ions decrease in the solution. It also means that the conversion increased with
time. For 100, 150 and 200 RPM, the conductivity remain almost constant as can be seen in the
graph. The same solution for 50 RPM is used for other RPMs. At 50 RPM, maximum conversion
has been reached, hence explain why the conductivity and conversion of solution for 100,150 and
200 RPM remain constant. It can be concluded that the conversion is inversely proportional to the
conductivity of the solution.
8
Theoretically, the higher the stirrer speed, more collision of molecules will occur hence the
conversion rate will increase. However, it is not guaranteed that higher rotating speed increase the
conversion, as it might not lead to perfect mixing. Rather at stirring speeds that are too fast, a lower
conversion will be achieved because a vortex will form in the solution causing splashes of
reactants to the reactor’s walls. This leads to inaccurate results and the reactants will have lesser
contact time with each other or residence time to react and lower chances of effective collision.
Thus, effective reaction will have lower tendency to occur. Therefore, an optimum rotating speed
need to be determined and applied so that it will only create turbulence for the mixing of reactants
to occur and not form a vortex. To avoid the generation of vortex, alternating impellers or two
reverse impellers can be used.
For this experiment, the relationship between the conversion or conductivity and rotational
speed cannot be deduced as the same solution is used for different RPM. The solution should be
replaced with other solution of the same concentration before changing the RPM of the stirrer.
Through this way, we can get more accurate results of the conductivity and conversion of the
solution and how they are affected by rotational speed. Hence, the optimal rotational speed for the
saponification reaction can be obtained.
Determining the Reaction Order and Rate Constant, k
From the experimental data, we can determine the order of reaction and the rate constant,
k. Zeroth order, first order and second order graphs are plotted in order to determine the correct
order of reaction. The rate constant, k, can be determined from the slope of the graph. The
concentration of sodium hydroxide at a given time can calculated using the following equation:
CA = CA0 (1-X)
The plotted graph will be based on the integrated rate law below:
0th Order 1st Order 2nd Order

Integrated Rate Law CA = CA0 - kt ln
𝐶𝐴
= - kt 1 1
𝐶𝐴0 = + 𝑘𝑡
𝐶𝐴 𝐶𝐴0
Table 2: Integrated rate law table
9
Since all the conditions tested are for the same reaction, only graph of 50 RPM is plotted.
Ca vs Time
0.1
0.09
0.08
0.07
0.06
[NaOH]
0.05
0.04
y = -0.0027x + 0.0846
0.03
R² = 0.8928
0.02
0.01
0
0 2 4 6 8 10 12 14
Time (min)
Figure 5: Graph of CA vs Time (Zero Order)
10
ln (Ca/Cao) vs Time
0
0 2 4 6 8 10 12 14
-0.1
-0.2
ln (Ca/Cao)
-0.3
-0.4
-0.5
-0.6 y = -0.0389x - 0.1565

R² = 0.9279
-0.7
Time (min)
𝑪
Figure 6: Graph of ln 𝑪 𝑨 vs Time (First Order)
𝑨𝟎
1/Ca vs Time
20
18
16
y = 0.5698x + 11.497
14
R² = 0.956
12
1/Ca
10
0
0 2 4 6 8 10 12 14
Time (min)
𝟏
Figure 7: Graph of 𝑪 vs Time (Second Order)
𝑨
11
From Figure 5,6 and 7, we can make comparison to determine the order of the reaction.
The order of reaction can be determined by comparing the value of R2, as the higher the value of
R2 indicate that the data is close to the fitted regression line. After comparing the three graphs, it
can be concluded that the order of the reaction is second order as R2 = 0.956 is the highest. Hence,
the value of rate constant, k, is equal to 0.5698 L/mol.s.
ERRORS & RECOMMENDATION
1) Random error
One of the main causes of error in this experiment is due to the fluctuation of temperature.
The temperature in the batch reactor is not constant during the stirring. Therefore, the rate
of reaction is not stable. The recommendation for this error is to take a few the reading of
the temperature and get its average temperature to minimize the error. Besides, another
cause of random error is due to the presence of remaining chemicals in the batch reactor.
The water does not fill up completely in the tank when rinsing the batch reactor. Thus,
there are still some portion of the uncleaned retained chemicals left on the reactor before
the next experiment is carried out. This causes the concentration of the solution in the
reactor to become different than the expected concentration. The main solution to reduce
this error is to make sure the water level of the clean water fills above the reactor before
draining it out.
Apart from that, another source of random error is due to the human error during dilution
process. Parallax error could occur when reading the level of the solution during the
dilution of the NaOH solution to the desirable volume. Moreover, timing error also happen
in this experiment. When recording the reading using the SOLDAS Data Acquisition
System, the timer does not start immediately when the stirrer starts rotating. This delay the
recording time for the conductivity result. The recommendation for this error is to ensure
12
the recording button is clicked when the power button for the stirrer is pressed
simultaneously.
2) Systematic error
Systematic error is often caused by instrumental error, method error or personal error.
There are few systematic errors occur in this experiment. One of the most significant error
is due to the inconsistent rate of stirring. For example, the rpm of the stirrer is not exactly
at 200rpm. This cause the data to be slightly affected. Therefore, the experiment should be
repeated for more than once to get the average reading of the data. Besides, the weighing
machine is also too sensitive. When measuring the weight of NaOH powder, the reading
of the weighing machine is affected by the wind movement. Therefore, in order to correct
this error, the weighing process should be carried out in a vacuum container.
On the other hand, there is also heat loss in the batch reactor. This contributes to the
inaccuracy result of the rate of reaction. Thus, the batch reactor should be insulated to
reduce the amount of heat loss.
13
In conclusion, conductivity is exhibited due to the presence of ions in the solution. In this
case, it is shown by the hydroxide ions from sodium hydroxide. Based on the calibration curve of
conversion versus conductivity, conductivity is seen to decrease with higher conversion. This is
because when the conversion of sodium hydroxide is low, the concentration of hydroxide ions
remaining in the solution is higher. Hence, the conductivity is higher. On the contrary, conductivity
decreases when conversion of sodium hydroxide is higher forming sodium acetate which is a weak
base.
Based on the second part of this experiment, it can be concluded that the batch
saponification reaction of ethyl acetate and sodium hydroxide is a second order reaction. This is
because it gives a linear plot with the highest R2 value for the plot of 1/Ca versus time in all
operating conditions. This experiment was also conducted to measure the conductivity values of
various stirring rates at 50, 100, 150 and 200 rpm. It is found that the conductivity value at 200
rpm is the lowest. Since conductivity is inversely proportional to conversion, a low conductivity
value signifies that the conversion of reactants at 200 rpm is the highest. This is because higher
mixing speed creates turbulence which improves the collision of particles which promotes higher
chances for the reaction to take place. However, this relation is only obeyed till a certain limit for
stirring speed. This is because if the speed is too high, the residence time for reactants to collide
and react will reduce due to the formation of vortex and splashing of solution to the sides of the
reactor. This reduces the conversion of reactants, hence, increases the conductivity value due to
higher concentration of hydroxide ions remaining in the solution.
14
Das, Kuheli & Sahoo, Parashuram & Magapu, Sai Baba & Murali, N. & Swaminathan, Pradeep.
(2011). Kinetic Studies on Saponification of Ethyl Acetate Using an Innovative
Conductivity-Monitoring Instrument with a Pulsating Sensor. International Journal of
Chemical Kinetics. 19. 648-656. 10.1002/kin.20597.
Hye Ji Lee, D. H. (2018). Transition Phase Approach for Statistical Model in Multiphase Process.
Seoul: Elsevier.
Lima, N. M., Linan, L. Z., Farias, F. S., Manenti, F., Filho, R. M., Embiruçu, M., & Maciel, M.
R. W. (2014).Optimal Fuzzy Control of Batch Polymerization Reactors: Application to
PMMA Production for Biomedical Purposes. Computer Aided Chemical Engineering
24th European Symposium on Computer Aided Process Engineering, 799–804. doi:
10.1016/b978-0-444-63456-6.50134-4
Liu, S. (2017). Batch Reactor. Bioprocess Engineering, 139–178. doi: 10.1016/b978-0-444-
63783-3.00004-6
Pontiga, F., & Castellanos, A. (1996). Electrical conduction of electrolyte solutions in nonpolar
liquids. IEEE Transactions on industry applications, 32(4), 816-824.
UMich. (2019, October 2). Retrieved from

http://umich.edu/~elements/5e/asyLearn/bits/batch/index.htm
15
CHAPTER 6 APPENDIX
Part A: Preparation of the calibration curve for Conversion vs. Conductivity
Table 2: Preparation for Calibration Curve.
Conversion 0.00 0.25 0.50 0.75 1.00
18.31 16.23 14.09 11.56 9.21
18.25 16.29 14.10 11.58 9.17
18.24 16.28 14.08 11.55 9.15
18.23 16.28 14.06 11.55 9.13
18.23 16.25 14.08 11.55 9.13
Conductivity 18.23 16.24 14.05 11.55 9.11
(mS/cm) 18.21 16.24 14.11 11.59 9.08
18.11 16.23 14.05 11.60 9.13
18.11 16.24 14.05 11.60 9.13
18.15 16.22 14.04 11.55 9.11
18.10 16.26 14.05 11.61 9.13
18.12 16.27 14.11 11.55 9.10
Average
Conductivity 18.19 16.25 14.07 11.57 9.13
(mS/cm)
Table 3: Mass of NaOH and CH3COONa need according to the concentration of the solution.
Concentration (M) Mass of NaOH (g) Mass of CH3COONa (g)
0.025 1 3.402
0.050 2 6.804
0.075 3 10.206
Sample Calculation
1. Calculate the mass of Sodium Hydroxide, NaOH for 1L of 0.025M NaOH
MW of NaOH = 40 g/mol
Mass of NaOH = (0.025M)(40g/mol)(1L) = 1g NaOH
∴ To make 0.025M NaOH solution, dilute 1g of NaOH in 1L water
2. Calculate the mass of Sodium Acetate, CH3COONa for 1L of 0.025M CH3COONa

MW of CH3COONa = 136.08 g/mol
Mass of CH3COONa = (0.025M)(136.08g/mol)(1L) = 3.402g CH3COONa
∴ To make 0.025M CH3COONa solution, dilute 2.05g of CH3COONa in 1L water
16
Part B: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide
Table 4: Conductivity and Conversion Values for Batch Saponification Reaction.
Time Conductivity (mS/cm) Conversion
(min) 50 RPM 100 150 200 50 RPM 100 150 200
RPM RPM RPM RPM RPM RPM
1 17.41 14.38 14.08 14.03 0.1092 0.4407 0.4735 0.4790
2 16.66 14.33 14.09 14.04 0.1913 0.4462 0.4725 0.4779
3 16.16 14.28 14.07 13.99 0.2460 0.4517 0.4746 0.4834
4 15.81 14.25 14.04 14.00 0.2843 0.4550 0.4779 0.4823
5 15.43 14.23 14.06 14.03 0.3259 0.4571 0.4757 0.4790
6 15.18 14.22 14.05 14.00 0.3532 0.4582 0.4768 0.4823
7 15.01 14.13 14.02 14.00 0.3718 0.4681 0.4801 0.4823
8 14.86 14.15 14.00 14.04 0.3882 0.4659 0.4823 0.4779
9 14.74 14.13 14.08 14.02 0.4013 0.4681 0.4735 0.4801
10 14.59 14.11 14.07 14.03 0.4178 0.4703 0.4746 0.4790
11 14.51 14.07 14.05 13.98 0.4265 0.4746 0.4768 0.4845
12 14.43 14.04 14.01 14.05 0.4353 0.4779 0.4812 0.4768
Table 5: Integrated Rate Law plot for 50 RPM.

Time
Conversion CA ln (CA/CAo) 1/CA
(min)
1 0.1092 0.0891 -0.1157 11.2264
2 0.1913 0.0809 -0.2123 12.3655
3 0.2460 0.0754 -0.2824 13.2625
4 0.2843 0.0716 -0.3345 13.9721
5 0.3259 0.0674 -0.3943 14.8337
6 0.3532 0.0647 -0.4357 15.4609
7 0.3718 0.0628 -0.4649 15.9186
8 0.3882 0.0612 -0.4914 16.3456
9 0.4013 0.0599 -0.5131 16.7041
10 0.4178 0.0582 -0.5409 17.1749
11 0.4265 0.0573 -0.5560 17.4370
12 0.4353 0.0565 -0.5714 17.7072
17
Time
(min)
1 0.4407 0.0559 -0.5811 17.8804
2 0.4462 0.0554 -0.5909 18.0570
3 0.4517 0.0548 -0.6009 18.2371
4 0.4550 0.0545 -0.6069 18.3469
5 0.4571 0.0543 -0.6109 18.4209
6 0.4582 0.0542 -0.6129 18.4581
7 0.4681 0.0532 -0.6313 18.7997
8 0.4659 0.0534 -0.6272 18.7227
9 0.4681 0.0532 -0.6313 18.7997
10 0.4703 0.0530 -0.6354 18.8774
11 0.4746 0.0525 -0.6437 19.0346
12 0.4779 0.0522 -0.6499 19.1543

Time
(min)
1 0.4735 0.0526 -0.6416 18.9951
2 0.4725 0.0528 -0.6395 18.9557
3 0.4746 0.0525 -0.6437 19.0346
4 0.4779 0.0522 -0.6499 19.1543
5 0.4757 0.0524 -0.6458 19.0744
6 0.4768 0.0523 -0.6478 19.1142
7 0.4801 0.0520 -0.6541 19.2349
8 0.4823 0.0518 -0.6584 19.3162
9 0.4735 0.0526 -0.6416 18.9951
10 0.4746 0.0525 -0.6437 19.0346
11 0.4768 0.0523 -0.6478 19.1142
12 0.4812 0.0519 -0.6562 19.2755
18
Time
(min)
1 0.4790 0.0521 -0.6520 19.1945
2 0.4779 0.0522 -0.6499 19.1543
3 0.4834 0.0517 -0.6605 19.3571
4 0.4823 0.0518 -0.6584 19.3162
5 0.4790 0.0521 -0.6520 19.1945
6 0.4823 0.0518 -0.6584 19.3162
7 0.4823 0.0518 -0.6584 19.3162
8 0.4779 0.0522 -0.6499 19.1543
9 0.4801 0.0520 -0.6541 19.2349
10 0.4790 0.0521 -0.6520 19.1945
11 0.4845 0.0516 -0.6626 19.3982
12 0.4768 0.0523 -0.6478 19.1142
Sample Calculation
Below are the sample calculation for experiment Part B at 50 RPM
Time= 1 min
Conversion, x = 0.1092
CAo = 0.1 M NaOH
1. To find CA of each conversion
CA = CAo(1-x)
CA = (0.1)(1-0.1092) = 0.0891 M
2. Zeroth-order reaction
CA = CAo – kt
plot graph of CA vs. t
slope of CA vs. t graph= -k
for zeroth-order reaction at 50 RPM

slope, -k = -0.0027
rate constant, k = 0.0027 mol L-1 min-1
19
3. First-order reaction
ln CA = ln CAo – kt
ln (CA/CAo) = -kt
plot graph of ln (CA/CAo) vs. t
slope of ln (CA/CAo) vs. t graph = -k
for first-order reaction at 50 RPM

slope, -k = -0.0027
rate constant, k = 0.0027 min-1
4. Second-order reaction
1 1
=𝐶 + 𝑘𝑡
𝐶𝐴 𝐴𝑜
1
plot graph of 𝐶 vs. t
𝐴
1
slope of 𝐶 vs. t graph = k
𝐴
for second-order reaction at 50 RPM

slope, k = 0.0012
rate constant, k = 0.0012 L mol-1 min-1
20
CDB 3052
SEPTEMBER 2019
Experiment : 6 – Sedimentation Studies Apparatus

Group : 1A
Phong Yue Jin 25197
Lab Instructor : Tan Hong Li
Date : 27th September 2019
Table of Contents
CHAPTER 1 INTRODUCTION & OBJECTIVES .................................................................... 3-5
CHAPTER 2 METHODOLOGY / EXPERIMENTAL PROCEDURE ...................................... 6-8
CHAPTER 3 RESULTS & DISCUSSION .................................................................................... 9
Experiment A: Effect of different initial heights and concentrations on the settling rate ..... 9-13
Experiment B: Effect of different volume of flocculants on the settling rate ...................... 14-16
ERRORS & RECOMMENDATIONS ..................................................................................... 16
CHAPTER 6 APPENDIX............................................................................................................. 19
2
INTRODUCTION
Sedimentation is a process that is widely used for wastewater treatment. Sedimentation
occurs when a dilute slurry is settled by gravity or when the slurry has a higher solid concentration
making it denser than the fluid (Geankoplis, 1993). The suspended particle in a solution will settle
down and form a barrier or layer usually located at the bottom of the container. The driving force
for sedimentation are due to gravity, centrifugal acceleration and even the difference in density of
the solid and liquid contents (McGraw-Hill, 2005).
The gravity settling rate would be very low if the solids in a suspension are mainly
individual particles (McCabe, 1993). To enhance the settling rate, flocculating agents are added.
Flocculation is carried out by adding materials such as alumina which form loose agglomerates
that carry fines down with flocculating agents. The agglomerated particles act like a single large
particle so that they settle at a feasible rate and leave a clear liquid behind (McGraw-Hill, 2005).
Figure 1: Batch sedimentation

Settling is the process where suspended particles settle through the liquid while
sedimentation marks the end of the settling process itself. There are several stages in a batch
sedimentation process. Different zones are formed along the sedimentation process. As shown in
Figure 1a, the solid is uniformly distributed in the liquid at the beginning of the batch
3
sedimentation process. After a while, the suspension is segregated into 4 zones. The solids that
have settled to give a zone of clear liquid, zone A, original suspension concentration zone, zone
B, transition layer, zone C, and a zone of settled solids, zone D as illustrated in Figure 1b. As the
settling continues, the depth of zone A and zone D increases while the depth of zone B decrease
whereas the depth of zone C remains nearly constant. This shown in Figure 1c. Eventually, zone
B disappears and all the solids are in the zone C and zone D. At the same time, the gradual
accumulation of the solids at the bottom will act as a force which compresses the settled solids at
the bottom of zone D and this moment is called a critical point. The compression forces the
remaining liquid in Zone A to spurt into other layers as shown in Figure 1d. The settling process
will stop when the weight of the solid is balanced by the compressive strength of the flocs. This
marks the end of the sedimentation process where the settling process has stopped as illustrated in
Figure 1e.
OBJECTIVE
The main objective of this experiment is to study the different characteristic of
sedimentation. This is done by studying the effect of different initial heights and concentrations
on the settling rate of corn starch in water and the effect of different volume of flocculants on the
settling rate of the corn starch in water.
1. Experiment A: Study of the effect of different initial heights and concentrations on the
settling rate
From Experiment A, the experiment is conducted with different initial height and
concentration of corn starch solution to study its effect on the settling rate. This is done by
preparing two different concentration of solution which are 50g of corn starch in 2L water and
100g of corn starch in 2L water. 5 cylindrical columns is then filled with the solution by varying
the initial height of the solution which are 90cm, 90cm, 60cm, 60cm and 30cm respectively. Each
column has different concentration where for cylinder column 1, cylinder column 3 and cylinder
column 3 are filled with 50g of corn starch in 2L water solution while the others are filled with
100g of corn starch in 2L water. Next, the height of clear liquid interface of each column is
measured for every 5 minutes interval for one hour. From the height of the clear interface for each
4
time interval, the settling rate of each column is determined. The effect of different initial heights
and concentrations on the settling rate is discussed after the experiment has completed.
2. Experiment B: Study of the effect of different volume of flocculants on the settling rate
For Experiment B, the same preparation of material as in Experiment A is prepared.
Flocculant solution is prepared by mixing 2g of Aluminium Oxide in 100ml water. Different
volumes of flocculants of 5ml, 10ml, 15ml, 20ml and 25ml are added to each of the cylinder
column respectively. The solution is stirred in each cylindrical column for the solid to be uniformly
distributed in the liquid. Next, the height of clear liquid interface of each column is measured for
every 5 minutes interval for one hour. From the height of clear interface for each time interval, the
settling rate of each column is determined. The effect of different volume of flocculants on the
settling rate is discussed after the experiment has completed.
5
CHAPTER 2 METHODOLOGY / EXPERIMENTAL PROCEDURE
Apparatus: Cylinders, beakers, stopwatch, beaker
Material : Corn starch, distilled water, Alum
General Start-up Procedure
1. Prepare corn starch solution in a plastic beaker. Remove the cylinder cap and slowly pour
the solution into the cylinder.
2. Hold the top and middle section of the glass cylinder and pull the cylinder carefully away
from the back panel.
the sentences must be in past principle
3. Plug the power cord into a power socket. tense!..
Experiment procedure
Experiment A: To determine the settling rate for different initial heights and concentrations.
1. The cylinders are emptied before starting the experiments. The top and the middle section
of the glass cylinder is held to empty the cylinders and the cylinder is pulled carefully away
2. Five different sets of corn starch solutions are prepared as follows:
a) Cylinder 1
Concentration: 50g of corn flour in 2L of water
Z0: 90 cm
b) Cylinder 2
Z0: 90 cm
c) Cylinder 3
Z0: 60 cm
d) Cylinder 4
Z0: 60 cm
e) Cylinder 5
Z0: 30 cm
6
3. The cylinder cap is removed and the solution is poured slowly into the cylinder. The
diagram is shown in figure 2.
Figure 2: Set up of the experiment.

4. The power cord is plugged into a power socket to turn on the back-panel illumination.
5. The solution in each cylinder is stirred until a uniformly distributed solid in the liquid is
achieved.
6. The initial time, t0, is recorded.
7. The height of the clear liquid interface, Z, is recorded at every 5 minutes intervals until the
settling process stops.
8. The final time, tf, is recorded.
9. The final heights, Zf. is recorded for each cylinder.
Experiment B: To determine the settling rate for different volume of flocculants.

1. The cylinders are emptied before starting the experiments. The top and the middle section
of the glass cylinder is held to empty the cylinders and the cylinder is pulled carefully away
2. The flocculent is prepared by mixing 20g of Aluminum Oxide (Alum) in 1L of water.
3. Five different sets of corn starch solutions are prepared as follows:
a) Cylinder 1
7
Z0: 90 cm
Flocculant: 5ml
b) Cylinder 2
Z0: 90 cm
Flocculant: 10ml
c) Cylinder 3
Z0: 60 cm
Flocculant: 15ml
d) Cylinder 4
Z0: 60 cm
Flocculant: 20ml
e) Cylinder 5
Z0: 30 cm
Flocculant: 25ml
4. The cylinder cap is removed and the solution is poured slowly into the cylinder.
5. The power cord is plugged into a power socket to turn on the back-panel illumination.
6. The solution in each cylinder is stirred until a uniformly distributed solid in the liquid is
achieved.
7. The initial time, t0, is recorded.
8. The height of the clear liquid interface, Z, is recorded at every 5 minutes intervals until the
settling process stops.
9. The final time, tf, is recorded.
10. The final heights, Zf. is recorded for each cylinder.
8
Experiment A: Effect of different initial heights and concentrations on the settling rate
In the 1st part of this experiment, various concentrations of corn starch are mixed into the
water (100g and 50g) with initial heights of different levels (90cm, 60cm and 30cm). Then, the
graph of height of clear liquid interface, Z versus settling time, t is plotted for the records of height
with 1 minute intervals for an hour.
Height of Clear Liquid Interface vs. Settling Time

4.00
3.50
Height of Clear Liquid Interface, Z (cm)
y = 0.0565x + 0.1286
3.00
y = 0.0437x + 0.1187
y = 0.0491x - 0.1912
2.50
y = 0.0434x - 0.189
2.00
1.50
y = 0.028x - 0.156
1.00
0.50
0.00
0 10 20 30 40 50 60 70
-0.50
Settling time, t (min)
50g, 90cm 100g, 90cm 50g, 60cm 100g, 60cm

100g, 30cm Linear (50g, 90cm) Linear (100g, 90cm) Linear (50g, 60cm)
Linear (100g, 60cm) Linear (100g, 30cm)
Figure 3: The graph of height of clear liquid interface versus settling time for various
concentrations and initial height.
As seen in figure 3, the height of clear liquid interface rises with time. This is due to the
occurrence of sedimentation where particles such as corn starch settle downward in the tube due
to it being denser than water. At the start of this experiment, the height of clear liquid interfaces
are recorded as 0 cm this is due to the initial mixing of corn starch in water which causes the solids
9
to be uniformly distributed in liquid. Hence, it is assumed that sedimentation has yet to occur. At
the initial part, approximately 5 min and below, the graphs of each variation of initial height (90
cm and 60 cm) for different concentration of corn starch showed overlapping lines. This is because
during the early stages, the settling rate is constant whereby the settling rate is judged by the
steepness of the slopes. At the beginning, the velocity of settling is slower because the particles
are still separated and small in sizes. This is followed by a steeper increase in the height of clear
liquid interfaces due to the different settling rates of different concentrations and initial height.
This is generally due to the dynamic motion of particles which attract one another. These forms
particles of larger clusters resulting in a denser solid and faster settling velocity (Kourki, 2011).
As the time reaches 60 minutes, the settling rates start to slow down shown by the less steep slopes
at the later stage of sedimentation. This is due to the large particle sizes which causes particle
collisions and frictional forces (Kourki, 2011) also known as hindered settings. Hence, this stops
the particles from settling down easily and the velocity of sedimentation becomes slower. From
another point of view, as more solids accumulate in the transition zone C, it is more difficult for
the solids to force out the water below the interface height because the path of water flow becomes
narrower. Towards the later stage of sedimentation, the disappearance (at a later settling time) of
zone B which is the zone below the clear liquid interface and above the transition zone C causes
the settling velocity to slow down. Hence, the settling rate will slowly decrease until an ultimate
height is reached. The ultimate height is when the weight of settled solids is balanced by the
compressive strength of the flocs signifying the end of the sedimentation process.
10
4.00
3.50 y = 0.0565x + 0.1286

3.00
y = 0.0437x + 0.1187
2.50 y = 0.0491x - 0.1912
2.00
y = 0.0434x - 0.189
1.50
1.00
0.50
0.00
0 10 20 30 40 50 60 70
-0.50
50g, 90cm 100g, 90cm 50g, 60cm 100g, 60cm

Linear (50g, 90cm) Linear (100g, 90cm) Linear (50g, 60cm) Linear (100g, 60cm)
Figure 4: The graph of height of clear liquid interface versus settling time for various
concentrations of corn starch dissolved in water (100g and 50g).
By comparing the graphs of a fixed 90 cm initial height, for 50 g and 100 g corn starch, the
settling rate is higher for 50 g at 0.0565 cm/min compared to for 100 g at 0.0437 cm/min. The
same relation is shown for 60 cm initial height at 50 g and 100 g of corn starch where the settling
rates are 0.0491 cm/min and 0.0434 cm/min respectively. Hence, it can be concluded that at a
lower concentration, the rate of sedimentation is higher.
This is because at higher suspension concentration, the inter-particle distance is smaller.

Thus, the thermodynamic forces acting on these particles are stronger (Kourki, 2011).
Subsequently, the particles have higher tendency to attract one another forming larger networks
leading to the reduction of sedimentation velocity. This can also be explained by the occurrence
of hindered settling of solid particles due to the high concentration of particles. This results in
11
increasingly significant inter-particle interactions or collision of particles increase
(Krishnamoorthy, 2010). Thus, due to the overcrowding of particles, the frictional forces at the
surface of particles also rise causing the decrease in settling velocities.

3.00
y = 0.0437x + 0.1187
2.50
2.00 y = 0.0434x - 0.189
1.50 y = 0.028x - 0.156
1.00
0.50
0.00
0 5 10 15 20 25 30 35 40 45 50 55 60 65
-0.50
100g, 90cm 100g, 60cm 100g, 30cm

Linear (100g, 90cm) Linear (100g, 60cm) Linear (100g, 30cm)
Figure 5: The graph of height of clear liquid interface versus settling time for initial heights (90
cm, 60 cm and 30 cm) for a fixed concentration.
Since this sedimentation experiment is carried out in vertical tubes, the main factors that
contribute to the variation in settling rate is the diameter of tube and initial height of fluid besides
the concentration of fluid (Galaez, n.d.). Generally, at the beginning, the effect of intial height of
suspension is not significant. However, at the later stages of sedimentation or at large scale
sedimentation, the sludge layers become thicker. Hence, the compression effects due to initial
suspension height is notable.
12
From Figure 5, the settling rate is almost the same for the initial suspension height of 90
cm and 60 cm at 0.0437 cm/min and 0.0434 cm/min respectively while it it is lower for 30 cm at
0.028 cm/min. This shows that there is a slight relation where as the height of suspension increases,
the settling rate increases as supported by Madhusan (2015). Overall, based on the first two
conditions, the settling rate for different initial suspension heights is almost the same. Thus, the
effect of initial height on the settling rate is minor. This is because the concentration of corn starch
is the same, hence the collision rate of particles is also the same. As for the initial height of 30cm,
the rate is significantly lower compared to the other two. This could be due to the hindered settling
effect caused by the overcrowding of particles in a smaller space making it collide more often.
This creates a frictional force restricting the downward movement of particles to settle.
13
Experiment B: Effect of different volume of flocculants on the settling rate
In the 2nd part of the experiment, aluminium hydroxide with 5ml, 10ml, 15ml, 20ml and
25ml are added into the corn starch solution respectively to act as the flocculant. The 5 cylinders
with similar corn starch concentration as the 1st part of the experiment was used.
Height of Clear Liquid Interface vs Settling Time

4.00
y = 0.0625x + 0.0511
3.50
3.00 y = 0.0474x + 0.0407

y = 0.0484x + 0.0055
2.50
y = 0.0432x - 0.0456
2.00
y = 0.0332x - 0.0225
1.50
1.00
0.50
0.00
0 10 20 30 40 50 60 70
-0.50
50g, 90cm 100g, 90cm 50g, 60cm

100g, 60cm 100g, 30cm Linear (50g, 90cm)
Linear (100g, 90cm) Linear (50g, 60cm) Linear (100g, 60cm)
Linear (100g, 30cm)
Figure 6: Graph of Height of Clear Liquid vs Settling Time (Different Volume of Flocculant)
Based on the graph, C1, C2, C3, C4 and C5 are prepared the same way as experiment 1.
The trend of the graph is similar to experiment 1 but the rate of sedimentation has increased slightly
due to the presence of flocculant. In the previous experiment before adding the flocculant, C2
(100g, 90cm) has lower rate of sedimentation compared to C5 (50g, 60cm) because C2 has higher
concentration. However, the rate of sedimentation for C2 (100g, 90cm) and C5 (50g, 60cm) are
almost the same in this experiment. This can be explained by the different volume of flocculant
added where 10ml of flocculant is added to C2 while 25ml of flocculant is added to C5. Therefore,
the rate of sedimentation increases when the volume of flocculant added increases. Flocculation
14
increases the particle size from sub microscopic micro floc to visible suspended particles called
flocs (Tzoupanos & Zoubolis, 2008). The particles then bind together and coagulate. This increases
their mass hence forming larger particles which settle faster and are resistant to break-ups in
turbulent areas.

2.50
y = 0.0332x - 0.0225
2.00
1.50
1.00
y = 0.028x - 0.156
0.50
0.00
0 10 20 30 40 50 60 70
-0.50
C5 (25ml Flocculant) C5 Linear (C5 (25ml Flocculant) ) Linear (C5 )
Figure 7: Graph of Height of Clear Liquid vs Settling Time (Comparing rate of

sedimentation of C5 before and after adding flocculant)
In this graph, C5 is selected to find out the effect of flocculant on the sedimentation rate.
Based on the graph, the trend is the same where the height of clear liquid is proportional to the
sedimentation time. The presence of 25ml flocculant decreases the sedimentation time where C5
(25ml flocculant) requires 30 minutes to achieve the height of clear liquid of 1cm whereas C5
requires 40 minutes to achieve the same height. Initially, the rate of sedimentation for both
experiments increases linearly. As time progresses, the rate of sedimentation decreases. This
phenomenon is due to the crowding of solid particles as the particles moves towards the bottom of
the cylinder by the pull of gravity force. Thus, it creates resistance to their downward motion.
15
Another perspective can be taken that as solids accumulate in zone C, the transition layer, it
becomes more difficult for the solids to push out the water below the interface height since the
path in which water can passthrough becomes narrower. (Camarote, Romelo and Valdon, 2017).
ERRORS & RECOMMENDATIONS
1. Random Error
One error encountered is the inconsistency in the mixing force of corn flour solution which
could cause solution to have incomplete mixing. Thus it is proposed that an automatic stirrer should
be used to ensure constant and uniform mixing of the solution. Besides that, readings and
measurements are not accurately taken. Therefore, it is recommended to use a ruler to align the
scale and liquid height to improve precision. Readings can also be taken every 5 minutes when
measuring the height of liquid with cautious and alertness. Eye level should be perpendicular to
the scale of reading.
2. Systematic Error
During experiment, there is an unclear liquid interface height which may be due to the lack
of color contrast with the back-panel illumination. Hence, a distinct and suitable light color should
be used instead to give a sharper contrast in the interface height. Moreover, zero error can be
prevented by placing the weighing scale in a closed container to avoid disturbance by external
factors such as air movement.
16
For the first part of the experiment (Part A), the objective is to study the effect of different
concentration and initial heights on the settling rate. At 90 cm initial height, for 50 g and 100 g
corn starch, the settling rate is higher for 50 g compared to 100 g. The same relation is shown for
60 cm initial height, where the settling rate for 50 g corn starch is higher. From the results obtained,
it can be concluded that at a lower concentration, the rate of sedimentation is higher. This is
because at higher suspension concentration, the sedimentation velocity is smaller because the
particles have higher tendency to attract one another forming larger networks. For the corn starch
with the same concentration at different initial heights, the settling rate obtained is almost the same.
This shows that initial height has minor effect on the settling rate. This is because the concentration
of corn starch is the same, hence the collision rate of particles is also the same.
For the second part of the experiment (Part B), the objective is to determine the effect of
different volumes of flocculants (aluminium hydroxide) on the settling rate. The results show that
the settling rate of all cylinders increase as the flocculants are added increases. This is because
flocculants promote flocculation that bind particles together and coagulate. This increases their
mass hence forming larger particles which settle faster and are resistant to break-ups in turbulent
areas. In the previous experiment before adding the flocculants, C2 (100g, 90cm) has lower rate
of sedimentation compared to C5 (50g, 60cm) because C2 has higher concentration. However, the
rate of sedimentation for C2 (100g, 90cm) and C5 (50g, 60cm) are almost the same in this
experiment. This can be explained by the different volume of flocculants added where 10ml of
flocculants is added to C2 while 25ml of flocculants is added to C5. It can be concluded that the
rate of sedimentation increases when the volume of flocculants added increases.
17
Camarote, B., Romelo, N., & Valdon, S. (2017). Batch Sedimentation. Retrieved from
https://www.academia.edu/33189302/Batch_Sedimentation
Galaez, D. M. R. (n.d.). Exp 4 Sedimentation. Retrieved from
https://www.scribd.com/document/343755476/Exp-4-Sedimentation
Geankoplis, C. J. (1993). Transport processes and unit operations (3rd ed.). Prentice Hall.
Kourki, H., & Famili, M.H. N. (2012). Particle sedimentation: effect of polymer concentration
on particle–particle interaction. Powder Technology, 221, pp. 137-143. Retrieved from
https://reader.elsevier.com/reader/sd/pii/S0032591011007339?token=1AEFD7899ACB5
5E5CAE4A3B3393AE63E847E45A4A109C346081725F8AA52EDD13BF6D9526909A
03941822ED54D84A1B0
Krishnamoorthy, P. (2010). Sedimentation model and analysis for differential settling of two -
particle - size suspensions in the Stokes region. International Journal of Sediment, pp.
119-133. Retrieved from
https://www.sciencedirect.com/science/article/pii/S1001627910600327
Madhusudan, V. (2015). What is the effect of an increase in height on the rate of sedimentation
of particles? Retrieved from https://www.quora.com/What-is-the-effect-of-an-increase-
in-height-on-the-rate-of-sedimentation-of-particles
McCabe, W. L., Smith, J. C., & Harriott, P. (1993). Unit operations of chemical engineering.
New York, NY: McGraw-Hill.
McGraw-Hill. (2005). McGraw-Hill concise encyclopedia of engineering. New York: McGraw-
Hill Education.
Soediono, B. (1989). Sedimentation. Journal of Chemical Information and Modeling, 53, 160
18
CHAPTER 6 APPENDIX
Table 1: Records of data to study the effect of different initial height and concentration on the
settling rate.
Z(cm)
Time (min) Cylinder 1 Cylinder 2 Cylinder 3 Cylinder 4 Cylinder 5
0 0.00 0.00 0.00 0.00 0.00
5 0.50 0.40 0.20 0.15 0.10
10 0.60 0.50 0.30 0.25 0.15
15 0.90 0.75 0.35 0.30 0.20
20 1.30 1.00 0.60 0.45 0.30
25 1.50 1.15 0.90 0.80 0.35
30 1.90 1.50 1.25 1.10 0.50
35 2.20 1.75 1.50 1.30 0.80
40 2.60 2.00 1.80 1.50 1.00
45 2.80 2.20 2.10 1.90 1.20
50 3.00 2.40 2.40 2.10 1.30
55 3.10 2.45 2.50 2.20 1.45
60 3.30 2.50 2.75 2.40 1.55
Table 2: Records of data to study the different volume of flocculants on the settling rate.
Z(cm)
Time (min)
Cylinder 1 Cylinder 2 Cylinder 3 Cylinder 4 Cylinder 5
0 0.00 0.00 0.00 0.00 0.00
5 0.30 0.20 0.15 0.10 0.10
10 0.70 0.50 0.40 0.30 0.20
15 1.00 0.70 0.70 0.60 0.40
20 1.30 1.00 0.95 0.80 0.65
25 1.60 1.30 1.30 1.10 0.90
30 1.95 1.50 1.60 1.30 1.00
35 2.30 1.80 1.80 1.50 1.30
40 2.60 2.00 2.10 1.80 1.40
45 3.00 2.30 2.20 1.90 1.50
50 3.20 2.40 2.40 2.05 1.60
55 3.50 2.60 2.60 2.30 1.70
60 3.60 2.70 2.75 2.50 1.90
19
CDB 3052
SEPTEMBER 2019
Experiment : 9 – Activated Carbon Adsorption (Task A)

Group : 1A
Phong Yue Jin 25197
Lab Instructor : Syeda Saba Fatima
Date : 20th September 2019
Table of Contents
CHAPTER 1 INTRODUCTION & OBJECTIVES .................................................................. 3 - 4
CHAPTER 2 METHODOLOGY / EXPERIMENTAL PROCEDURE .................................... 5 - 7
CHAPTER 3 RESULTS & DISCUSSION ............................................................................. 8 - 14
Part A: To achieve 70% removal efficiency of methylene blue using activated carbon as an
adsorbent .............................................................................................................................. 8 - 10
Part B: Determine the adsorption isotherm and its respective isotherm constant ................ 10-15
CHAPTER 6 APPENDIX...................................................................................................... 18 - 25
2
INTRODUCTION
Methylene blue is a synthetic basic colouring compound commonly found in discharges
from textile, cosmetics and food processing industries into rivers, lakes and drainage systems.
Compared to its uses, the threat it possess towards the environment is critical. One of the reasons
is because the contaminated water will inhibit the penetration of sunlight into the water affecting
the photosynthesis process of aquatic plants which then disrupts the overall marine ecosystem.
However, methylene blue is a synthetic complex organic aromatic structure making it inert and
tough to bio-degrade (Samal, 2014). Hence, multiple strategies have been applied in solving this
issue including ion exchange, biological treatments, chemical coagulation and more (Gecgel et al.,
2012). Among the alternatives, the most effective approach is by activated carbon adsorption due
to its high adsorption capacity, possibility to regenerate, sludge free operation, micro pores
structures and large surface area (Samal, 2014; Obuge, 2014).
Adsorption is defined as the attachment of molecules to a surface (toppr, n.d.). It involves

the substance adsorbed which is the adsorbate and the substance it is adsorbed to which is the
adsorbent. This process is mainly affected by the selectivity of the adsorbent towards the adsorbate,
the operating temperature and pressure. The adsorption rate increases with the rise in pressure due
to compression of adsorbates on the adsorbent and the drop of temperature that favours the forward
reaction. Adsorption can also be categorized based on the forces of attraction between the
adsorbent and adsorbate. Physical adsorption involves weak Van der Waals forces whereas in
chemical adsorption there are strong chemical bonds. In this experiment, the adsorption of
methylene blue onto activated carbon does not involve a reaction nor is heating required as
activation energy, hence, this process is denoted as physical adsorption.
In the adsorption of dye molecules, it is crucial to select an adsorbent that is able to contain
a large amount of adsorbate and is recyclable (Ghaedi et al., 2014). Based on effectiveness,
activated carbon which is a carbonaceous material derived from charcoal, commonly in the form
of very fine powder or granules is chosen. This is due to its high affinity towards various dyes,
microporous structure (high ratios of surface area over weight up to 100 acres per pound) and a
large adsorption capacity. Not only that, it can also be regenerated by heating to release the
attached molecules on adsorbent based on Le Chatelier’s principle. Currently, there are many
3
variations for activated carbon from local agricultural origin such as coconut shell and sugarcane
which effectively lowers the operating cost and is easily obtainable (Ghaedi et al., 2014).
OBJECTIVES
The main objective is to study the fundamental behaviour of adsorption by using activated
carbon. This covers the equilibrium isotherms, adsorption kinetics and operational characteristics
of an activated carbon adsorption system. This is done by studying the effect of the mass of
adsorbent on its removal efficiency and determining the adsorption isotherm it adheres to. s
to what?
Part a: Study of the effect of mass of adsorbent on the removal efficiency of methylene blue
from the solution.
For part a, the experiment is conducted to achieve at least 70% removal efficiency of
adsorbate (methylene blue) using activated carbon. This is done by fixing the concentration of
methylene blue at 30 mg/L and varying the mass of activated carbon at 3g, 6g and 9g. Then, the
activated carbon is each mixed in a beaker of 30 mg/L methylene blue respectively. Next, the
absorbance of light by the solution is measured using a UV-Vis spectrometry for fixed time
intervals. From the calculated concentration for each time interval, the amount of activated carbon
which required the shortest time to achieve 70% removal efficiency is determined and used as the
sample for part b of this experiment.
Part b: Determination of the best fit adsorption isotherm and its respective isotherm
constants for the adsorption of methylene blue by activated carbon.
Using the mass of activated carbon determined in part a, the solution of methylene blue
varying from 10 mg/L to 30mg/L are mixed with the adsorbent respectively. The solutions are
tested for their absorbance values at constant time intervals until a constant reading is achieved.
This indicates that the equilibrium condition is reached and the adsorbent is almost or at its
saturation capacity. Hence, the values at equilibrium are used to plot the Langmuir and Freundlich
plot to determine which isotherm best fits the adsorption process. Its isotherm constants are
calculated from the linearized form of each empirical equation.
4
CHAPTER 2 METHODOLOGY / EXPERIMENTAL PROCEDURE
Apparatus: UV visible spectrophotometer, stirrer machine, electronic weighing balance, 1L

beaker, 1L volumetric flask, spatula, vial
Material : Activated granular R&M Chemicals, methylene blue powder, distilled water
General Start-up Procedure
1. UV visible spectrophotometer is turned on and warmed up for 15 minutes.
2. A vial is filled with distilled water and inserted into spectrophotometer.
3. Zero button is pushed to calibrate the spectrophotometer.
4. The spectrophotometer is run with wavelength of 465nm.
Experiment procedure
Part A: To obtain 70% removal efficiency of methylene blue using activated carbon.
1. General start-up procedure is performed to calibrate the UV visible spectrophotometer.
2. 0.03g of methylene blue powder is weighted using electronic weight balance and diluted
with distilled water and poured into 1L volumetric flask.
3. The volumetric flask is filled with distilled water until the calibration point.
4. The volumetric flask is closed and shook well.
5. The solution is poured into 1L beaker.
6. Step 2-5 is repeated twice to prepare another 2 beakers of 1L of methylene blue solution.
7. Three different vials is filled up with 10ml of three samples of methylene blue solution
from each beaker and the initial absorbance is measured using spectrophotometer.
8. The initial absorbance of each samples is recorded.
9. The beakers of methylene blue solution is put under the agitators of stirrer machine and the
machine is operated at 250 RPM.
10. 3g, 6g and 9g of activated granular R&M chemicals is weighted using electronic weighing
balance.
11. 3g, 6g and 9g activated carbon is added into the beaker respectively and the timer is started
simultaneously.
12. 10 mL of methylene blue solution is put into a clean and dry vial for every 5 minutes
intervals and for each solution.
5
13. The absorbance of the samples is measured 3 times and the average values is recorded.
14. The samples is poured back into their original solution in the beakers.
15. The vials is cleaned with distilled water and the vials is dried.
16. The percent removal efficiency is calculated and recorded.
i. The calibration plot for methylene blue is formed by plotting the graph of
absorbance versus concentration of methylene blue (mg/L). The data is taken from
the absorbance of distilled water and methylene blue at 10 mg/L, 20 mg/L and 30
mg/L at time, t = 0 minute.
ii. The concentration of methylene blue (mg/L) is calculated by using the equation of
the trendline from the calibration plot where the y = absorbance and x =
concentration of methylene blue (mg/L).
iii. The value of concentration of methylene blue calculated at each absorbance is
substituted into the following formula:
17. Step 12-16 is repeated and stopped after one of the three samples reaches 70% removal
efficiency of methylene blue solution.
Part B: To determine the adsorption isotherm and adsorption constant using activated carbon
1. General start-up procedure is performed to calibrate the UV visible spectrophotometer.
2. Three samples of Activated granular R&M Chemicals that first achieve the 70% removal
efficiency in Part A is weighted using electronic weight balance.
3. 0.01g, 0.02g and 0.03g of methylene blue powder is weighted using electronic balance and
diluted with distilled water and poured into three different 1L volumetric flask.
4. The volumetric flask is filled with distilled water until the calibration point.
5. The volumetric flask is closed and shook well.
6. The solution is poured into 1L beaker.
7. Three different vials is filled up with 10ml of three samples of methylene blue solution
from each beaker and the initial absorbance is measured using spectrophotometer.
6
8. The initial absorbance of each samples is recorded.
9. The beakers of methylene blue solution is put under the agitators of stirrer machine and the
machine is operated at 250 RPM.
10. The activated carbon weight earlier is added into each beaker respectively and the timer is
started simultaneously.
11. 10 mL of methylene blue solution is put into a clean and dry vial for every 5 minutes
intervals and for each solution.
12. The absorbance of the samples is measured 3 times and the average values is recorded.
13. The samples is poured back into their original solution in the beakers.
14. The vials is cleaned with distilled water and the vials is dried.
15. The concentration of methylene blue is calculated and recorded.
i. The calibration plot for methylene blue is formed by plotting the graph of
absorbance versus concentration of methylene blue (mg/L). The data is taken from
the absorbance of distilled water and methylene blue at 10 mg/L, 20 mg/L and 30
mg/L at time, t = 0 minute.
ii. The concentration of methylene blue (mg/L) is calculated by using the equation of
the trendline from the calibration plot where the y = absorbance and x =
concentration of methylene blue (mg/L).
16. Step 11-15 is repeated and stopped after the reading of absorbance of all three samples
remains constant.
17. The adsorption isotherm is determined by plotting the graphs using Freundlich and
Langmuir isotherms and which graph results in a linear plot is determined.
18. The adsorption constant of methylene blue solution is calculated after the adsorption
isotherm is determined.
19. Equilibrium concentration of methylene blue absorbed onto activated carbon, qe is
calculated by using the value of equilibrium concentration of methylene blue, ce.
7
Part A: To achieve 70% removal efficiency of methylene blue using activated carbon as
an adsorbent
In this experiment, the methylene blue solution acts as the adsorbate while activated carbon
acts as the adsorbent. In the first part of the experiment, different masses of activated carbon which
consist of 3g, 6g, and 9g are added to three 1L sample of 30mg/L of methylene blue solution
respectively. The absorbance reading of methylene blue solution is recorded for every 5 minutes
interval until 70% efficiency is attained.
Calibration Plot for Methylene Blue

0.3
y = 0.0091x - 0.0058
R² = 0.9934
good
0.25
0.2
Absorbance
0.15
0.1
0.05
0
0 5 10 15 20 25 30 35
-0.05
Concentration of methylene blue, Ct (mg/L)
Figure 3.1 Calibration Curve of Methylene Blue Solution at 465nm.

The calibration curve is established from the absorbance values of different concentration
of methylene blue solution (10mg/L, 20mg/L, 30mg/L) and distilled water by referring to part b
of this experiment. Figure 3.1 shows the line has regression coefficient of 0.9934 which is near to
the unity. Therefore, the absorbance value is directly proportional to the concentration of
methylene blue solution. This calibration plot is used to determine the concentration of methylene
blue based on the absorbance value measured from each interval by using the trendline equationS.
8
Removal Efficiency Vs Time
90.000
80.000
Removal Efficiency (%)

70.000
60.000 3g
Carbon
50.000
6g
40.000 Carbon
30.000 9g
20.000 Carbon
10.000
0.000
0 10 20 30 40 50 60
good plotting but its better to
Time, t (min) show the reading in the graph
from 70%...
Figure 3.2 Removal Efficiency of Methylene Blue Against Time using Different Mass of
Activated Carbon
Based on the graph, 9g carbon is the first to reach the 70% removal efficiency at the 16th
min, followed by 6g carbon which takes 22min to reach 70% removal efficiency. However, the 3g
carbon does not reach removal efficiency of 70% because the total surface area available for
adsorption is fully occupied before it can reach 70% efficiency. This result can be accepted because
the solute removal efficiency increases as the mass of adsorbent increases. The increase in
adsorbent mass increases the contact surface of adsorbent particles which means that it will be
more probable for solute molecules to be adsorbed on adsorption sites, and thus adsorption
efficiency is increased (O.F. Okeola et al, 2011). In fact, the rate of adsorption is affected by the
mass of adsorbent used. The rate of adsorption will be higher if more than 9g of carbon is used.
From the trend of the graph above, the removal efficiency of the methylene blue increases
with time and eventually reach a constant value for all the different mass of carbon. The main
reason that the removal efficiency reaches a constant value is because the adsorption site is fully
filled with methylene blue particles. As methylene blue particles contact with the carbon adsorbent.
The methylene blue solutes slowly fill up some of the available sites. As time passes, the active
region decreases until it is fully occupied. Thus, the adsorption process stops once all the active
site of carbon adsorbent is fully occupied, the removal efficiency remains constant. In this
experiment, the graph illustrates that the time taken for 6g and 9g carbon to reach a constant value
of removal efficiency is at 25 minutes. However, the removal efficiency of the 3g carbon still
9
increase slightly until the end of the experiment. Theoretically, the 3g carbon should be the 1 st to
reach the constant value of removal efficiency since the total surface area for adsorption site is the
lowest and followed by 6g carbon and 9g carbon. This error occurs due to systematic error such
as irregular rate of mixing of the agitator.
The rate of adsorption of methylene blue from the activated carbon is influenced by the
temperature of the solution. The adsorption capacity of the activated carbon increased with
decreasing of the temperature. Since adsorption is an exothermic reaction, this indicates that the
adsorbates release energy when attached to the surface of adsorbent. Hence, based on Le
Chatelier’s principle, the decrease in temperature will favour the forward reaction causing a higher
rate of adsorption. On the other hand, increasing the pressure will directly increase the rate of
adsorption. When the pressure increases, the frequency of collision of the methylene blue particle
will collide more frequently with the active site of carbon. When the capacity of adsorption
achieves the maximum, the adsorbent can either be replaced or regenerated so that the percentage
of solutes removed can be higher.
Part B: Determine the best fit of adsorption isotherm and its respective isotherm constant
In this part of the experiment, the mass of activated charcoal is fixed at 9 gram, while the
concentration of methylene blue is varied at 10mg/L, 20mg/L and 30mg/L. The absorbance
readings are taken from each sample of different concentration until a constant value is obtained,
whereby equilibrium condition is achieved. The concentration corresponding to the constant
absorbance reading is known as equilibrium concentration. With the equilibrium concentration of
solution, Ce and equilibrium concentration of adsorbates adsorbed onto adsorbents, qe, the
linearized isotherm expressions are represented graphically. This method of linearizing isotherm
is a good and reasonable way to determine if the isotherm best describe the equilibrium behavior
of experimental data (Chen, 2015). The experimental data collected is plotted as shown in Figure
3.3.
10
Concentration of methylene blue vs Time
10mg/L 20mg/L 30mg/L
Concentration of methylene blue, ct 35.000

30.000
25.000
20.000
(mg/L)
15.000
10.000
5.000
0.000
0 10 20 30 40 50
Time, t (min)
Figure 3.3 Concentration of Methylene Blue Against Time at Constant Mass of Activated
Carbon
From the experimental results shown in Figure 3.3, it can be observed that the
concentration of methylene blue decreases with increasing time until equilibrium is achieved,
where concentration of methylene blue is constant. This is because the solute particles of
methylene blue solution adsorb onto the surface of activated carbon, thus lowering the
concentration of methylene blue solution. Since the surface of activated carbon is empty initially,
the rate of adsorption is higher. This may be attributed to the higher concentration gradient as the
driving force (Bassim H. Hameed, 2007). As time prolongs, the rate of adsorption decreases shown
by slower decreasing rate of methylene blue concentration. This is due to adsorption being a
reversible reaction, thus desorption also occur to oppose the changes in adsorption, according to
Le Chatelier’s principle (McDermott, 1971). At equilibrium, the rate of adsorption and rate of
desorption are constant, thus the concentration of methylene blue is constant. The equilibrium
concentration of 30mg/L methylene blue solution is the highest, since it has the highest initial
concentration with the same amount of activated charcoal as that in 10mg/L and 20mg/L
methylene blue concentration.
With the experimental data, the linearized model of Freundlich and Langmuir isotherms
are plotted to see which model best fit the equilibrium behavior of this experimental results. Figure
3.4 shows the Freundlich plot.
11
Freundlich plot - ln of equilibrium concentration of adsorbate
on adsorbent vs. ln of equilibrium concentration of solute,
ln qe vs. ln ce
adsorbate on adsorbent, ln qe (mg/g)

ln of equilibrium concentration of 1.200
y = 3.53x - 5.6309
0.800 R² = 0.9396
0.400
0.000
1.300 1.400 1.500 1.600 1.700 1.800 1.900 2.000
-0.400
-0.800
-1.200
ln of equilibrium concentration of solute, ln ce (mg/L)
Figure 3.4 Freundlich plot: Graph of the ln of equilibrium concentration of adsorbate on

adsorbent versus the ln of equilibrium concentration of solute, ln qe vs. ln Ce
From Figure 3.4, the R2 value obtained from the line is relatively high, which is 0.9396.
This implies that the isotherm can explain 93.96% of the set of data. The straight-line graph shows
a positive slope. The gradient value is 3.53 and the y-intercept value is -5.6309. From the intercept,
the Freundlich constant (KF) is calculated and its value is 3.585 × 10−3 mg/g. KF is the indication
of adsorption capacity and its value is considerably low. Besides that, the intensity of adsorption
(1/n) is calculated and the n-value is 0.283g/L.
Several assumptions were taken into consideration during the adsorption process so that
the Langmuir isotherm can be fitted. These assumptions include:
1. The adsorption sites are uniform and only one molecule could be adsorbed into each site.
2. No interaction between adsorbed molecules.
3. The adsorbates remain at the active site until desorption occurs.
4. At maximum adsorption, only monolayer of adsorbate is formed at the surface of
adsorbent.
Figure 3.5 shows the Langmuir plot.
12
Langmuir Isotherm - lnverse of equilibrium concentration of
adsorbate on adsorbent vs. lnverse of equilibrium
concentration of solute, 1/qe vs. 1/ce
lnverse of equilibrium concentration of

adsorbate on adsorbent , l/qe (g/mg)
2.500
2.000
1.500 y = -15.382x + 9.8558
R² = 0.6508
1.000
0.500
0.000
-0.5000.400 0.500 0.600 0.700 0.800
-1.000
-1.500
-2.000
lnverse of equilibrium concentration of solute, 1/ce (L/mg)
Figure 3.5 Langmuir Isotherm: Graph of the inverse of equilibrium concentration of adsorbate on
adsorbent versus inverse of equilibrium concentration of solute, 1/qe vs. 1/Ce
From Figure 3.5, the linearized form of Langmuir isotherm is plotted by 1/qe versus 1/Ce,
and the R2 value obtained from the line is considerably low at 0.6508, implying that the isotherm
can explain 65.08% of the set of data. The graph shows a negative gradient value of -15.382 and a
y-intercept value of 9.8558. The value of adsorption capacity (KL) and the theoretical monolayer
saturation capacity (qm) are calculated using the Langmuir Isotherm formula. The value of KL is -
0.6405 L/mg and the maximum concentration of adsorbate adsorbed on adsorbent, qm is
0.1015mg/g. The negative value of KL suggests two possible explanations, which are either
Langmuir isotherm is not the best fitted model or considerably significant errors were made during
the experiment.
Based on the analysis of Freundlich and Langmuir isotherms, Freundlich isotherm seem to
be the more suitable model to fit this experimental data. The R2, which represents the similarity
index to the raw data of the experiment, is higher for Freundlich isotherm than that for Langmuir
isotherm. Moreover, the negative value of Langmuir constant, KL implies that Langmuir isotherm
is not a suitable model to fit the data. Furthermore, the linearized graphical plot for Freundlich
isotherm generates a straight-line graph, while Langmuir gives a curve. Hence, it can be concluded
that Freundlich isotherm is the suitable model for this experiment.
13
ERRORS & RECOMMENDATION
1. Random error
Random error is errors that caused by natural phenomena and cannot be controlled by
human. The weighing balance is very sensitive and can be easily affected by the
surrounding air in the laboratory. The recommendation to solve this error is to close the
cover of the weighing balance before taking readings and take average reading of the
weight. There is also parallax error in reading the level of solution in the volumetric flask.
Hence, the level of observation should be directly perpendicular to the level of solution
when reading the volume and an average reading from multiple trails can help reduce this
error.
Next, the dilution of methylene blue powder was not done accurately. The distilled water
added for one of the volumetric flasks exceeded the calibration mark and there was some
residue of the methylene blue solution in the beaker that was not fully transfer into the
volumetric flask. This error caused the concentration of methylene blue to deviate from its
desired concentration. Therefore, the recommendation to solve this error is to make sure
all methylene blue is well transfer into the volumetric flask by washing the beaker with
distilled water repeatedly and transferring it into the volumetric flask. A dropper should be
used to add distilled water into the volumetric flask when the solution about to reach the
calibration mark.
2. Systematic error
Systematic errors are errors that are caused by either technique, instruments or even
procedures of the experiment itself. In this experiment, there were a few systematic errors
that occurred. Firstly, the stirring machines that are used for the experiment are operated at
different stirring rates for every beaker containing methylene blue solution. It ranges from
240 RPM to 300 RPM causing variation in adsorption rate. This caused some of the
activated carbon to be settled at the bottom of the beaker and not well mixed. Hence, to
solve this error, a stirrer machine with multiple agitators should be used to make sure the
14
speed of the agitators are all the same and a glass rod in-hand to mix any excess activated
carbon that settled at the bottom or the wall of the beaker.
Next, the starting time of each machine is different leading to different timer used for each
beaker. Since three different stirrer machines are used, the three “on” switches need to be
push simultaneously. However, due to the machines’ faultiness, the stirrers of the beakers
did not move simultaneously causing variation in the starting time of stirring for each
solution. There was an agitator of a different brand that had a slower starting rate of stirring
which varies the results obtained. This might cause some error in the absorbance readings
since the stirrer does not set at the same time. To solve this error, the recommendation is
to use a stirrer machine with multiple agitators so that the agitators will start simultaneously
and the timer for all beaker will be the same.
Lastly, the reading of the absorbance varies for the same sample. The reading of the
spectrophotometer changed for the same sample each time. This could be due to the
faultiness of the cuvette or vial used due to the scratches and fingerprint marks left on the
transparent sides. This affects the travel of light through the sample causing inaccurate
readings. The recommendation to solve this error is to take average reading of each sample
and use a better conditioned cuvette.
15
For the first part of the experiment (Part A), three different masses of activated carbon
which consist of 3g, 6g, and 9g is added to three 1L samples of 30 mg/L methylene blue solution
respectively. The objective of this experiment is to achieve 70% removal efficiency of methylene
blue. The results show that 6g and 9g activated carbon manage to attain at least 70% removal
efficiency. This conforms that the solute removal efficiency increases as the mass of adsorbent
increases, because the contact surface between adsorbent and adsorbate increases, hence the
removal efficiency increases. After some time, the removal efficiency remains constant, indicating
that the adsorption process stops because the active site of carbon adsorbent is fully occupied. The
results of this experiment show that methylene blue solution with 6g and 9g activated carbon reach
the constant value of removal efficiency faster than 3g. Theoretically, the smaller the weight of
activated carbon, the faster the time to reach constant value of removal efficiency as the total
surface area for adsorption site is smaller. Due to the systematic error such as irregular rate of
mixing of the agitator, the results obtained are not aligned to the theory.
For the second part of the experiment (Part B), constant mass of activated carbon of 9g is
added to three 1L samples of methylene blue solution with the concentrations are varied at 10mg/L,
20mg/L and 30mg/L. The aim of this experiment is to determine the best fit of adsorption isotherm
and its respective isotherm constant. The linearized model of Freundlich and Langmuir isotherms
are plotted from the data obtained and the constants for each isotherm is calculated. For Freundlich
isotherm, the calculated constant (KF) is 3.585 x 10-3 mg/g and as for the Langmuir isotherm, the
calculated constant value (KL) is -0.6405 L/mg. The results indicate that Freundlich isotherm is
more suitable to fix this experimental data. This is because the R2 value for Freundlich is higher,
the Freundlich constant (KF) obtained is positive, and the graph generated is a straight-line graph.
16
Bassim H. Hameed, A. L. (2007). Adsorption of Basic Dye (Methylene Blue) onto Activated
Carbon Prepared from Rattan Sawdust. Dyes and Pigments, 143-149.
Chen, X. (2015). Modeling of Experimental Adsorption Isotherm Data. Information, 14-22.
Gecgel, U., Ozcan, G., & Gurpinar, G. C. (2013). Removal of Methylene Blue from Aqueous
Solution by Activated Carbon Prepared from Pea Shells (Pisum sativum). Journal of
CHemistry, 1-9. https://doi.org/10.1155/2013/614083
Ghaedi, M., Golestani Nasab, A., Khodadoust, S., Rajabi, M., &Azizian, S. (2014). Application
of activated carbon as adsorbents for efficient removal of methylene blue: Kinetics and
equilibrium study. Jounral of Industrial and Engineering Chemistry, 2317-2324.
McDermott, K. E. (1971). Absorption and desorption accompanied by a reversible reaction.
American Institute of Chemical Engineers, 536-541.
Obuge, Macaulay, A., Evbuomwan, & B, O. (2014). Adsorption of Methylene Blue

onto Activated Carbon Impregnated with KOH using Cocoa Shells. IJETR, 11-
18.
Samal, D. P. (2014). Characterization and study of adsorption of methylene blue dye using
activated carbon. Retrieved from http://ethesis.nitrkl.ac.in/5710/1/110CH0108-7.pdf
toppr. (n.d.). Adsorption. Retrieved from https://www.toppr.com/guides/chemistry/surface-
chemistry/adsorption/
17
CHAPTER 6 APPENDIX
(Part a)
Table 1: Values of absorbance of methylene blue at concentration 0 mg/L, 10 mg/L, 20 mg/L and
30 mg/L, t=0 (This data is used to construct the calibration curve).
Concentration of methylene blue (mg/L) Absorbance
0 0
10 0.072
20 0.184
30 0.265
Table 2: Values of absorbance, concentration of methylene blue and removal efficiency for 3g
activated carbon.
Time (min) Absorbance Concentration of Removal Efficiency
methylene blue, Ct (%)
(mg/L)
0 0.304 34.044 0.000
5 0.221 24.923 26.791
10 0.195 22.066 35.184
15 0.164 18.659 45.190
20 0.176 19.978 41.317
25 0.165 18.769 44.868
30 0.160 18.220 46.482
35 0.154 17.560 48.418
40 0.149 17.011 50.032
45 0.133 15.253 55.197
50 0.130 14.923 56.165
55 0.128 14.703 56.811
activated carbon.
(mg/L)
0 0.290 32.505 0.000
5 0.225 25.363 21.974
10 0.160 18.220 43.949
15 0.127 14.593 55.105
18
20 0.093 10.857 66.599
25 0.071 8.440 74.037
30 0.070 8.330 74.375
35 0.070 8.330 74.375
40 0.067 8.000 75.389
45 0.059 7.121 78.093
50 0.061 7.341 77.417
55 0.064 7.670 76.403
activated carbon.

(mg/L)
0 0.301 33.714 0.000
5 0.261 29.319 13.038
10 0.167 18.989 43.677
15 0.094 10.967 67.471
20 0.069 8.220 75.619
25 0.050 6.095 81.921
30 0.043 5.399 83.985
35 0.046 5.656 83.225
40 0.045 5.582 83.442
45 0.043 5.363 84.094
50 0.043 5.363 84.094
55 0.043 5.363 84.094
19
Sample Calculation
• Calculate the concentration of methylene blue at any given time, Ct.
Using the equation of the trendline from the calibration plot, the concentration of methylene
blue (mg/L) can be calculated.
The line equation from the calibration plot:
y= 0.0091x – 0.0058
where
y = absorbance
x = concentration of methylene blue (mg/L).
For methylene blue solution with 3g activated carbon at 25 minutes,
y=0.165
x= 18.769 mg/L
Ct= 18.769 mg/L
• Calculate the removal efficiency at any given time.
Using the following formula, the removal efficiency can be calculated.
For methylene blue solution with 3g activated carbon at 25 minutes,

C0= 34.044 mg/L
Ct= 18.769 mg/L
Removal efficiency = 44.868%
20
(Part b)
Table 5: Values of absorbance, concentration of methylene blue, Ct and the concentration of
adsorbate on adsorbent, qt for 10 mg/L methylene blue solution taken with 5 minutes intervals.
Concentration of methylene
Concentration of
Time, t blue absorbed onto activated
Absorbance methylene blue, C
(min) carbon, qt
(mg/L)
(mg adsorbate / g adsorbent)
0 0.072 8.549 0.000
5 0.068 8.110 0.049
10 0.052 6.352 0.244
15 0.048 5.912 0.293
20 0.040 5.033 0.391
25 0.036 4.593 0.440
30 0.032 4.154 0.488
35 0.032 4.154 0.488
40 0.032 4.154 0.488
45 0.032 4.154 0.488

Concentration of
(min) carbon, qt
(mg/L)
0 0.184 20.857 0.000
5 0.095 11.077 1.087
10 0.079 9.319 1.282
15 0.061 7.341 1.502
20 0.053 6.462 1.599
25 0.049 6.022 1.648
30 0.044 5.473 1.709
35 0.043 5.363 1.722
40 0.043 5.363 1.722
45 0.043 5.363 1.722

21
Concentration of
(min) carbon, qt
(mg/L)
0 0.265 29.758 0.000
5 0.169 19.209 1.172
10 0.120 13.824 1.770
15 0.090 10.527 2.137
20 0.076 8.989 2.308
25 0.057 6.901 2.540
30 0.056 6.791 2.552
35 0.055 6.681 2.564
40 0.055 6.681 2.564
45 0.055 6.681 2.564
Table 8: Data of initial concentration, C0 and calculated values of equilibrium concentration, Ce

and equilibrium concentration of adsorbate on adsorbent, qe for 0.01 g, 0.02 g and 0.03 g of
methylene blue solution.
Initial
Equilibrium Equilibrium concentration of
Mass of concentration of
concentration of methylene blue absorbed onto
methylene methylene blue,
methylene blue, Ce activated carbon, qe
blue, m (g) C0
(mg/L) (mg adsorbate/g adsorbent)
(mg/L)
0.01 8.549 4.154 0.488
0.02 20.857 5.363 1.722
0.03 29.758 6.681 2.564
Table 9: Calculated values for Freundlich and Langmuir plot.
Mass of methylene blue, m ln ce ln qe 1/ce 1/qe

(g) (mg/L) (mg/g) (L/mg) (g/mg)
0.01 1.424 -0.717 0.702 -1.394
0.02 1.680 0.543 0.595 1.840
0.03 1.899 0.942 0.527 1.062
Sample Calculation
• Determine the concentration of methylene blue adsorbed onto activated carbon at
any given time, qt.
22
𝑉
𝑞𝑡 = (𝐶0 −𝐶𝑡 ) ×
𝑚
where C0 = initial concentration of methylene blue, Ct = concentration of methylene blue
adsorbed onto activated carbon at time, t, V = volume of solution, m = mass of activated
carbon
For 10 mg/L methylene blue solution at 25 minutes,

- The volume of solution, V for this experiment is set as 1 L.
- The Ct = 4.593 mg/L and C0 = 20.857 mg/L
- The mass of activated carbon used for this experiment (part b) is 9 g.
1
𝑞𝑡 = (20.857 − 4.593) × 9
= 0.440 𝑚𝑔/𝐿
• Determine the concentration of methylene blue adsorbed onto activated carbon at

equilibrium, qe.
𝑉
𝑞𝑒 = (𝐶0 −𝐶𝑒 ) ×
𝑚
where C0 = initial concentration of methylene blue, Ce = concentration of methylene blue
adsorbed onto activated carbon at equilibrium, V = volume of solution, m = mass of
activated carbon
For 10 mg/L methylene blue solution,

- The volume of solution, V for this experiment is set as 1 L.
- Since equilibrium is reached when the absorbance shows a constant reading, hence,
Ce = 4.154 mg/L
- C0 = 20.857 mg/L
- The mass of activated carbon used for this experiment (part b) is 9 g.
1
𝑞𝑒 = (20.857 − 4.154) × 9
= 0.488 𝑚𝑔/𝐿
23
Calculate the isotherms constants for Freundlich and Langmuir isotherms.
• Freundlich Isotherm
1) Linearize the empirical equation describing Freundlich isotherm.
Empirical equation:
1
𝑞𝑒 = 𝐾𝐹 × 𝐶𝑒𝑛
where qe = equilibrium concentration of adsorbate on adsorbent, Ce = equilibrium
concentration of solute, KF and n = experimental constants
Linearize by placing “ln” on both sides of the equation:

1
𝑙𝑛𝑞𝑒 = 𝑙𝑛𝐾𝐹 + 𝑙𝑛𝐶𝑒
𝑛
2) Obtain the values of slope and y-intercept from the Freundlich plot and calculate
the isotherm constants.
From Figure 3, the slope of the Freundlich plot is y = 3.53x-5.6309 where y = ln qe and x
= ln Ce.
Therefore,
1
Gradient = 𝑛 = 3.53
n = 0.283 g/L
y-intercept = ln KF = -5.6309
KF = 𝑒 −5.6309
= 3.585 × 10−3 mg/g
• Langmuir Isotherm
1) Linearize the empirical equation describing Langmuir isotherm.
Empirical equation:
𝑞𝑚𝑎𝑥 𝐾𝐿 𝐶𝑒
𝑞𝑒 =
1 + 𝐾𝐿 𝐶𝑒
24
where qe = equilibrium concentration of adsorbate on adsorbent, qmax = maximum
concentration of adsorbate on adsorbent, Ce = equilibrium concentration of solute, KL =
experimental constant.
Linearize the equation:

1 1 1
= +
𝑞𝑒 𝑞𝑚𝑎𝑥 𝐾𝐿 𝐶𝑒 𝑞𝑚𝑎𝑥
2) Obtain the values of slope and y-intercept from the Langmuir plot and calculate the
isotherm constants.
From Figure 4, the slope of the Langmuir plot is y = -15.382x + 9.8558 where y = 1/qe
and x = 1/Ce.
Therefore,
y-intercept = 1/𝑞𝑚 = 9.8558

𝑞𝑚 = 1/9.8558
= 0.1015 mg/g
1
Gradient = = -15.382
𝐾𝐿 𝑞𝑚𝑎𝑥
1
= -15.382
𝐾𝐿 (0.1015)
1
KL =
−15.382 ×0.1015
KL = -0.6405 L/mg
25

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CDB 3052

CHEMICAL ENGINEERING LABORATORY (II)

Experiment : 2 – Plug Flow Tubular Reactor

CHAPTER 1 INTRODUCTION & OBJECTIVES ....................................................................... 3

CHAPTER 2 METHODOLOGY ................................................................................................... 5

CHAPTER 3 RESULTS & DISCUSSION .................................................................................... 8

ERRORS & RECOMMENDATIONS ................................................................................................... 15

CHAPTER 5 REFERENCES ....................................................................................................... 17

(1) No mixing in the axial direction

NaOH + CH3COOC2H5 → CH3COONa + C2H3OH

1. To prepare the calibration curve for conversion versus conductivity

Material: Sodium Hydroxide, Ethyl Acetate, Water

Figure 1: The unit set up for plug flow reactor

1. The following solutions is being prepared:

General Shut-down Procedures

Part A: Preparation of Calibration Curve for Conductivity vs Conversion

1. The calibration curve of conductivity vs conversion of saponification reaction of ethyl

Part B: Saponification of Et(Ac) and NaOH in Plug Flow Reactor

1. The general start-up procedures are performed.

Figure 2: Graph of Conductivity vs Conversion

CH3COOCH2CH3 + NaOH → CH3COONa + CH3CH2OH

PART B: Batch Saponification Reaction of Ethyl Acetate and Sodium Hydroxide

−𝒓𝑨 = 𝒌𝑪𝑨 𝑪𝑩 = 𝒌𝑪𝟐𝑨

−𝒓𝑨 = 𝒌𝑪𝟐𝑨𝟎 (𝟏 − 𝑿)𝟐

Determination of reaction rate constant in terms of residence time

NaOH Et (Ac) Total Residenc Average Conver Fraction Reaction Rate

Residence Time vs. Total Feed Flowrate

Figure 3: Graph of Residence Time vs. Total Feed Flowrate

Average Outlet Conductivity vs. Residence Time

Figure 4 Graph of Average Outlet Conductivity vs. Residence Time

Conversion vs. Residence Time

Figure 5: Graph of Conversion of Ethyl Acetate vs. Residence Time

Reaction Rate Constant vs. Total Feed Flowrate

Rate of reaction, -rA (mol/L min)

−𝒓𝑨 = 𝒌𝑪𝟐𝑨𝟎 (𝟏 − 𝑿)𝟐

Conversion Solution Mixture (ml) Concentration Conductivity

2. Calculate the mass of Sodium Acetate, CH3COONa for 1L of 0.025M CH3COONa

Calculation of the volume of the plug flow reactor

Calculation of the residence time

The residence time can be calculated using the following equation:

𝐕𝐫𝐞𝐚𝐜𝐭𝐨𝐫 𝐕𝐨𝐥𝐮𝐦𝐞 𝐨𝐟 𝐫𝐞𝐚𝐜𝐭𝐨𝐫

After rearranging, the equation to find the conversion is as below:

For v0 = 0.1 L/min and average outlet conductivity, y = 6.562 mS/cm,

For v0 = 0.2 L/min and average outlet conductivity, y = 5.873 mS/cm,

For v0 = 0.3 L/min and average outlet conductivity, y = 6.551 mS/cm,

For v0 = 0.4 L/min and average outlet conductivity, y = 6.561 mS/cm,

For v0 = 0.5 L/min and average outlet conductivity, y = 6.812 mS/cm,

Calculation of the rate constant, k (L/mol.min)

The rate constant can be calculated from the following equation:

The reaction rate can be calculated using the following equation:

For v0= 0.2 L/min,

For v0= 0.3 L/min,

Experiment : 4 – Batch Liquid Reactor

CHAPTER 1 INTRODUCTION & OBJECTIVES .................................................................. 3

CHAPTER 3 RESULTS & DISCUSSION ................................................................................. 6

ERRORS & RECOMMENDATION ............................................................................... 12-13

CHAPTER 4 CONCLUSION .................................................................................................... 14

CHAPTER 5 REFERENCES .................................................................................................... 15