CRE Manual

LIST OF EXPERIEMNTS IN CHEMICAL RREACTION ENGINEERING (LAB)
1. Analyze the effect of concentration on the rate of a chemical reaction

2. Analyze the effect of Temperature on the Rate of a Chemical Reaction on varying
concentration reactant
3. Analyze the effect of surface area (particle size of a solid reactant) on heterogeneous
chemical reaction
4. Measure the conversion of saponification reaction in Batch reactor
5. Measure the conversion of saponification reaction in CSTR in series
6. Obtain the reaction order by integral method of data analysis.
7. Plot conversion as a function of concentration of reactants and products.
8. Determine the specific reaction rate constant.
9. Demonstrate that the saponification of the ethyl-acetate with sodium hydroxide is a
reaction of first order with respect to ethyl-acetate.
10. Demonstrate the dependency of the velocity constant with temperature obeying the law
of Arrhenius.
11. Determine experimentally the tubular reactor conversion.
12. Determine the conversion regarding the residence time.
13. Determination of the reaction order and the speed constant.
COURSE LEARNING OUTCOMES (CLOs)
The course learning outcomes for the mass transfer operations lab are presented below:
1. Describe the fundamentals of Chemical Reaction Engineering lab experiments and

associated lab equipment
2. Analyze the effect of different parameters on chemical reactions, working principle and
functions of major components of different lab-scale/industrial equipment related to the
subject lab
3. Perform all experiments by following standard operating procedure (SOP) and

troubleshooting protocols while operating any equipment
4. Demonstrate report writing and presentation skills while submitting any technical or
scientific report using latest computer aided tools in general and ones specific to chemical
engineering
5. Adopt safety measures to avoid any accident and be prepared for any unwanted event
during work
6. Commit to basic human or professional ethics and teamwork attributes
PROGRAMME LEARNING OUTCOMES (PLOs)

The programme learning outcomes are depicted as below:
1. Engineering Knowledge
2. Investigation
3. Modern Tool Usage
4. The Engineer and Society
5. Ethics
6. Individual and Teamwork
7. Communication
8. Lifelong Learning
Assessment Plan
Description Weightage CLOs Covered
Lab Rubric 1 5% 1,2,3,4,5,6
Lab Rubric 2 8% 1,2,3,4,5,6
Lab Rubric 3 / Open Ended 12% 1,2,3,4,5,6
Lab
Sessional 1 Examination 10% 1,2,3,4,5,6
Sessional 2 Examination 15% 1,2,3,4,5,6
Terminal Examination 20% 1,2,3,4,5,6
Safety Rules and Regulations
PRE-CHECKS:
Before starting any laboratory operation, ask and answer the following questions by
yourself:
1. Have I done this before?
2. Do I have the proper equipment?
3. Does anything look wrong?
4. What are the hazards?
5. Should I work in a fume hood?
6. Do I need goggles or other safety equipment?
7. Do I need additional help?
8. Should I check further with my instructor?
9. Have I planned this experiment or exercise?
10. Do I know what to do, if there is an accident?
11. Do I know where the fire extinguishers are located?

LABORATORY SAFETY RULES
1. NO SMOKING IS ALLOWED IN THE LABORATORY PREMISES.
2. Safety glasses must be worn at all times (where applicable) during laboratory periods.
These glasses should be kept between laboratory sessions in the racks provided.
3. Wear apron (lab overall) in the lab when running apparatus and handling liquids.
4. Wear rubber gloves when handling liquids.
5. When dangerous chemicals are in use, a second person should be within call.
6. Find out the location of First Aid Box.
7. Before operating any valve, switch, etc., know precisely what the effect of your
manipulation will be.
8. Turn off all the valves on cylinders of compressed or liquefied gases when not in use.
9. Students are not allowed to open gas cylinders. Ask the technician.
10. Report all injuries to the instructor and to COMSATS doctor immediately. Dial 1122.
11. Attach a label "Please leave on" on fittings, you need "on" for a long time.
12. Keep all inflammable liquids or gases away from open electrical equipment and other
sources of ignition.
13. Avoid inhalation of gases or vapors of any kind.
14. Do not leave cables trailing across the floor of the lab.
15. Practice good housekeeping. Clean all spills at once. Return all equipment to proper
storage when not in use. Place all trash in appropriate receptacles.
16. Make sure any system being heated is properly vented.
17. Know the location and use of all emergency, protective, and firefighting equipment.
18. Do not smell directly any chemical being heated.

19. Remember that, if a lab smells, do not use it. Inform instructor/lab technician.
20. Do not leave lab while apparatus is on, always inform the instructor if you are in a
situation to leave the lab.
21. When working with others, be especially careful not to drop tools.
22. Do not wear loose clothing or neckties when working with machinery. You will not
be allowed to enter the lab if you are in loose dress or not wearing covered shoes.
23. Report to the instructor any conditions that are safety hazards.
24. All power wiring is to be installed by an approved electrician.
25. Always remember: SAFETY IS GOOD TECHNIQUE!

Experiment # 1
Experiment Title: Analyze the effect of concentration.
Pre Lab(CLO1)
1.1 Objective:
Analyze the effect of concentration on the rate of a chemical reaction

1.2 Introduction
The purpose of this experiment is to determine the effect of changing the concentration of a
reactant upon the rate of a reaction. The reaction examined is that between sodium thiosulfate
and hydrochloric acid:
Na2S2O3 + 2HCl → 2 NaCl + H2O + S + SO2
The concentration of the thiosulfate will be changed by adding water and the appearance of the
opaque colloidal sulfur will be used to determine the rate of the reaction.
1.3 Description:
The effect of changing the concentration of thiosulfate ion is studied by observing the time
required for a fixed amount of product to form. As the reaction proceeds, the solution becomes
cloudy due to the formation of a colloidal dispersed precipitate of sulfur. In order to determine
the point at which a specific amount of product has formed, an "x" is observed through the
solution. The reaction is timed until the "x" is no longer visible.
1.4 Chemicals:
0.15 M sodium thiosulfate solution
6 M HCl solution
Equipment:
250-mL beakers
Stirring rods
25-mL graduated cylinder

Stop Watch, White paper.
1.5 HAZARDS
Concentrated solution of HC1 will burn skin or damage clothing; avoid skin contact with acid.
Reactions should be carried out in a well-ventilated room; some poisonous SO2 (g) is produced.
Students should be cautioned against leaning over reaction vessel too closely as they observe the
"x" under the beaker. Goggles should be worn throughout the experiment.
1.6 Procedure:
1. Obtain five 250-mL beakers, about 30 mL of hydrochloric acid solution, and about 80
mL of sodium thiosulfate solution. Label the beakers from 1 to 5. Add the amounts of
sodium thiosulfate solution and distilled or deionized water to each cup indicated in the
following Table 1.
2. Note that the total volume in each beaker is 25 mL.
3. Make a table that shows the information in the table above and also includes a column for
time (sec) and relative rate (sec-1).
4. Make a small "x" on a sheet of white paper with a pencil. Place a beaker containing the
sodium thiosulfate solution over this "x." Add 5 mL HCl solution and begin timing the
reaction as soon as the acid touches the sodium thiosulfate solution. Stir the reaction
mixture at a constant rate throughout the reaction.
5. Stop timing when the "x" under the beaker is no longer visible through the solution.
Record this time in your data table.
6. Repeat steps 2-4 for the remaining samples.
In-Lab (CLO # 3, CLO # 5, CLO # 6)
1.7 Safety Observations:

1. Do not run the service unit idle.
2. Ensure that storage tank is at least 80% full when you start the peristaltic pumps.
3. Ensure that at the end of the experimental performance, all parts of the service unit are closed.
4. Wear gloves and face masks as this experiment involves handling of chemicals.
5. Drain the reactors carefully.
6. Make sure the reactant solutions are prepared in distilled water in order to ensure the safety of
the reactor system.
1.8 Observations and Calculations:

Table 1.1
Vol. of Na2S2O3 Vol. of Volume and Time until cross disappearance.
solution (ml) distille Concentration of
d water sodium
Beakers
thiosulfate
1 25 0 100% (25ml)
2 20 5 80% (20ml)
3 15 10 60% (15ml)
4 10 15 40% (10ml)
5 5 20 20% (5ml)
Post-Lab (CLO # 2)
Findings
60
50
40
Time, (sec)
30
20
10
0
0.005 0.01 0.015 0.02 0.025 0.03 0.035 0.04 0.045 0.05 0.055
Concentration, (M)
Figure 1: Effect of concentration on rate of chemical reaction
Organization of lab reports

Point *1.1 to 1.5
Experiment # 2
Experiment Title: Analyze the effect of Temperature.
Pre Lab(CLO1)
2.1. Objective:
Analyze the effect of concentration on the rate of a chemical reaction

2.2 Introduction
The purpose of this experiment is to determine the effect of changing the temperature of a
reactant upon the rate of a reaction. The reaction examined is that between sodium thiosulfate
and hydrochloric acid:
Na2S2O3 + 2HCl → 2 NaCl + H2O + S + SO2
The concentration of the thiosulfate will be changed by adding water and the appearance of the
opaque colloidal sulfur will be used to determine the rate of the reaction.
2.3 Description:
The effect of changing the concentration of thiosulfate ion is studied by observing the time
required for a fixed amount of product to form. As the reaction proceeds, the solution becomes
cloudy due to the formation of a colloidal dispersed precipitate of sulfur. In order to determine
the point at which a specific amount of product has formed, an "x" is observed through the
solution. The reaction is timed until the "x" is no longer visible.
2.4 Chemicals:
0.15 M sodium thiosulfate solution
6 M HCl solution
Equipment:
250-mL beakers
Stirring rods
25-mL graduated cylinder

Stop Watch, White paper.
2.5 HAZARDS
Concentrated solution of HC1 will burn skin or damage clothing; avoid skin contact with acid.
Reactions should be carried out in a well-ventilated room; some poisonous SO2 (g) is produced.
Students should be cautioned against leaning over reaction vessel too closely as they observe the
"x" under the beaker. Goggles should be worn throughout the experiment.
2.6 Procedure:
1. Obtain five 250-mL beakers, about 30 mL of hydrochloric acid solution, and about 80
mL of sodium thiosulfate solution. Label the beakers from 1 to 5. Add the amounts of
sodium thiosulfate solution and distilled or deionized water to each cup indicated in the
following Table 1.
2. Note that the total volume in each beaker is 25 mL.
3. Make a table that shows the information in the table above and also includes a column for
time (sec) and relative rate (sec-1).
4. Make a small "x" on a sheet of white paper with a pencil. Place a beaker containing the
sodium thiosulfate solution over this "x." Add 5 mL HCl solution and begin timing the
reaction as soon as the acid touches the sodium thiosulfate solution. Stir the reaction
mixture at a constant rate throughout the reaction.
5. Stop timing when the "x" under the beaker is no longer visible through the solution.
Record this time in your data table.
6. Repeat steps 2-4 for the remaining samples.
2.7 Safety Observations:

6.Make sure the reactant solutions are prepared in distilled water in order to ensure the safety of
the reactor system.
Table 2.2
Vol. of Vol. of Volume and Time until cross Reaction Rate
Beakers
Na2S2O3 distille Concentration disappearance (1/time, sec-1)

solution d water of sodium (sec)
(ml) thiosulfate 35C 75C 35C 75C
1 25 0 100% (25ml)
2 20 5 80% (20ml)
3 15 10 60% (15ml)
4 10 15 40% (10ml)
5 5 20 20% (5ml)
Post-Lab (CLO # 2)
Findings
60
50
40
Time, (sec)
30
35C
20
60C
10
0
0 0.01 0.02 0.03 0.04 0.05 0.06
Concentration, (M)
Figure 2:Effect of concentration on rate of chemical reaction

Point *2.1 to 2.8
Experiment # 3
Experiment Title: Analyze the effect of surface area.
Pre-Lab (CLO # 1)
3.1. Objective:
Analyze the effect of surface area (particle size of a solid reactant) on

heterogeneous chemical reaction
3.2. Introduction:
If a chemical reaction involves one or more solid reactants, the particle sizes of the solid
reactants will affect the rate of the reaction. It is because surface area increases as the particles
become smaller. Increasing the reactants’ surface area allows the reactants approach to each
other more frequently, and so the reaction rates are often enhanced. A daily example is the
burning of charcoal. Powdered charcoal burns more fiercely than large lumps of charcoal. It is
because powdered charcoal has a much larger surface for reacting with oxygen.
Calcium carbonate reacts with diluted hydrochloric acid to give calcium chloride and carbon
dioxide gas. The rate of CO2 gas formation allows us to observe the reaction rate conveniently.
In this experiment we will compare the reaction rates of diluted hydrochloric acid with CaCO3
powder and CaCO3 granules.
You are going to collect and analyze data to find the order of this reaction with respect to
hydrochloric acid.
CaCO3(s) + 2HCl(aq) → CaCl2(aq) + CO2(g) + H2O(l)
The calcium carbonate you will use is in the form of marble. Fairly large pieces are used so that
the surface area does not change significantly during the reaction. However, the quantity and
concentration of hydrochloric acid is such that it is almost all used up during the reaction. Wear
eye protection and take care with the gas syringe.
3.3. Procedure:
1. 1 Set up the apparatus as shown in the diagram.

2. 2 Place about 10 g of marble in six or seven lumps in the test tube.
3. 3 Use a measuring cylinder to measure 10 cm3 of 1 M hydrochloric acid.
4. 4 Put the acid into the test tube. Allow a few seconds for the solution to become saturated
with carbon dioxide. Put the stopper in place and start timing.
5. 5 Take readings of volume (Vt) every 30 seconds, until the reaction is over and the
volume no longer changes. Record the final volume as well.
6. 6 When the reaction is over, the total volume of carbon dioxide collected (Vfinal) is
proportional to the concentration of the hydrochloric acid at the moment when timing
started. So (Vfinal – Vt) is proportional to the concentration of hydrochloric acid at each
time t. Complete the third column.
7. 7 Plot a graph of (Vfinal – Vt) against t, putting t on the horizontal axis.
8. Record your results in a table 3
3.4. Safety Observations:

the reactor system.
3.5. Observations and Calculations:
Table 3.3
Time (sec) Volume of Co2 (ml), Vt Vf-Vt (ml)
Figure 3:Schenatic diagram and result presentation to study effect of particle size on rate of chemical reaction
Post-Lab (CLO # 2)
Findings
Lab report Point 3.1 to 3.5
Experiment # 4
Experiment Title: Batch Reactor
Pre-Lab (CLO # 1)
4.1. Objective:
Measure the conversion of saponification reaction in Batch reactor
4.2. Process and Applications:
The Batch reactor is the generic term for a type of vessel widely used in the process industries. In
a batch reactor the reactants and the catalyst are placed in the reactor and the reaction is allowed
to proceed for a given time whereupon the mixture of unreacted material together with the
products is withdrawn. Provision for mixing may be required. In an ideal batch reactor, the
concentration and temperature are assumed to be spatially uniform. In practice, the condition can
be approximately realized by vigorous agitation or stirring. All the elements of the fluid spend
the same amount of time in the reactor, and hence have the same residence time.
Batch reactors are simple and needs little supporting equipment, and is therefore ideal for small
scale experimental studies on reaction kinetics. Industrially it is used when relatively small
amounts of material are to be treated and when the product demand varies. Batch reactors are
often used in the pharmaceutical industry, where small volumes of high-value products are made.
Researchers typically use a batch reactor to study reaction kinetics under ideal conditions. A
batch reactor can be used to find the reaction rate constant, activation energy and order of the
reaction. The data reflect the intrinsic kinetics for the reaction being investigated.
A typical batch reactor consists of a tank with an agitator and integral heating/cooling system.
Liquids and solids are usually charged via connections in the top cover of the reactor. Vapors
and gases also discharge through connections in the top. Liquids are usually discharged out of
the bottom.
The advantages of a batch reactor lies in its versatility. A single vessel can carry out a sequence
of different operations without the need to break containment. This is particularly useful when
processing, toxic or highly potent compounds.
Saponification of ethyl acetate using sodium hydroxide is carried out in a batch reactor. The
reaction is as follows:
CH3COOC2H5+ NaOH →CH3COONa + C2H5OH
The conversion of sodium hydroxide is calculated as:
X NaOH = ((CNaOH,o − CNaOH)/ CNaOH,o)*100%
Where CNaOH,o denotes the initial concentration and CNaOH is the concentration of sodium
hydroxide measured at the outlet.
The changing concentration of acetate and hydroxide ions has the most significant influence on
the total conductivity. As the reaction progresses, the acetate ions, with a less molar conductivity
replace the same number of hydroxide ions, which have a much higher molar conductivity. As a
result, the total conductivity proportionally decreases with the increasing conversion.
4.3. Experimental Procedure:
1. 500mL solution of NaOH with molarity of 0.03M and 500mL solution of ethyl acetate
having molarity of 0.05 were prepared.
2. Check all the electrical connections and flow lines.
3. Carefully switch on the electronic console and service unit with the help of command on
PC.
4. Provide the feed to reactor by attaching the inlet pipe of batch reactor to the containers
having NaOH and CH3COOC2H5 solutions (set the RPM of peristaltic pumps at 100 %.)
5. Reaction starts as soon as the reactants enter the batch reactor.
6. Keep on noticing the reading of conductivity of reaction mixture on monitor of PC.
7. As the reaction proceeds, concentration of NaOH will drop in the reaction mixture and so
is the value of conductivity.
8. Let the system run until no change in the value of conductivity is observed.
9. Use the table 4.1 in order to plot the concentration (x-axis) vs conductivity (y-axis) graph.
10. Complete the table 4.2 by using graph potted in step 9 (Write the values of concentration
against every reading of conductivity using the concentration vs conductivity graph)

the reactor system.
Table 4.4: Experimental Readings
No. of Concentration / Molarity of NaOH Conductivity

obs. solution (M) (µS/cm)
1 0.004 1000
2 0.005 1250
3 0.006 1500
4 0.007 1750
5 0.008 2000
6 0.009 2250
7 0.01 2500
No. of Time (min) Conductivity Concentration

obs. (µS/cm) (M)
1 0 1500
2 2 1480
3 4 1370
4 6 1370
5 8 1350
6 10 1350
7 12 1320
8 14 1320
9 16 1270
10 18 1260
11 20 1260
12 22 1260
Initial concentration of NaOH = CNaOH,o = 0.03M

Final concentration of NaOH = CNaOH = (final reading from table 4.2)
Find the conversion using formula:
Post-Lab (CLO # 2)
4.6. Findings
Concentration v/s Conductivity
7000
6000 f(x) = 203318.035093528 x + 287.655106770401

R² = 0.998230686804852
Conductivity (uS/cm) 5000
4000
3000
2000
1000
0
0 0.005 0.01 0.015 0.02 0.025 0.03 0.035
Concentration of NaOH (M)
Figure 4: Effect of concentration of NaOH on conductivity

4.7. Conclusion
result, the total conductivity proportionally decreases with the increasing conversion until it
becomes constant.
Organization of Lab Report (CLO # 4)
• Point # 4.1 to 4.7
Experiment # 5
Experiment Title: Continuous Stirred Tank Reactor
Pre-Lab (CLO # 1)
5.1. Objective:
Measure the conversion of saponification reaction in Continuous Stirred Tank Reactor
5.2. Process and Applications:
Continuous stirred tank reactors (CSTR) are the most basic of the continuous reactors used in
chemical processes. Continuous stirred-tank reactors (CSTRs) are open systems, where material
is free to enter or exit the system that operate on a steady-state basis, where the conditions in the
reactor don't change with time. Reactants are continuously introduced into the reactor, while
products are continuously removed.
CSTRs are very well mixed, so the contents have relatively uniform properties such as
temperature, density, etc. throughout. Also, conditions in the reactor's exit stream are the same as
those inside the tank. Systems connecting several CSTRs are used when the reaction is too slow.
Multiple CSTRs can also be used when two immiscible liquids or viscous liquids are present and
require a high agitation rate. CSTRs consist of a tank, usually of constant volume, and a stirring
system to mix reactants together. Also, feed and exit pipes are present to introduce reactants and
remove products. Fermenters are CSTRs used in biological processes in many industries, such as
brewing, antibiotics, and waste treatment. In fermenters, large molecules are broken down into
smaller molecules, with alcohol produced as a by-product.
Continuous stirred-tank reactors are most commonly used in industrial processing, primarily in
homogeneous liquid-phase flow reactions, where constant agitation is required. They may be
used by themselves, in series, or in a battery.
They are cheap to construct, have large capacity and interior of reactor is easily accessed.
Saponification of ethyl acetate using sodium hydroxide is carried out in a CSTR in series. The
reaction is as follows:
CH3COOC2H5+ NaOH →CH3COONa + C2H5OH
The conversion of sodium hydroxide is calculated in all reactors as follows:
Where CNaOH,o denotes the initial concentration and CNaOH is the concentration of sodium
hydroxide measured at the outlet.
result, the total conductivity proportionally decreases with the increasing conversion.
5.3. Experimental Procedure:
1. 10 L solution of NaOH with molarity of 0.02M and 10L solution of ethyl acetate having
molarity of 0.05 were prepared.
2. Check all the electrical connections and flow lines.
3. Carefully switch on the electronic console and service unit with the help of command on
PC.
4. Provide the feed to reactor by attaching the inlet pipe of first reactor to the containers
having NaOH and CH3COOC2H5 solutions (set the RPM of peristaltic pumps at 100 %.)
5. Reaction starts as soon as the reactants enter the batch reactor.
6. Keep on noticing the reading of conductivity of reaction mixture on monitor of PC.
7. As the reaction proceeds, concentration of NaOH will drop in the reaction mixture and so
is the value of conductivity in all the reactors.
8. Let the system run until no change in the value of conductivity is observed.
9. Use the table 5.1 in order to plot the concentration (x-axis) vs conductivity (y-axis) graph.
10. Complete the table 5.2 by using graph potted in step 9 (Write the values of concentration
against every reading of conductivity using the concentration vs conductivity graph)

11. Make sure the reactant solutions are prepared in distilled water in order to ensure the
safety of the reactor system.
No. of Concentration / Molarity of NaOH Conductivity

obs. solution (M) (µS/cm)
1 0.004 1000
2 0.005 1250
3 0.006 1500
4 0.007 1750
5 0.008 2000
6 0.009 2250
7 0.01 2500
Table 5.7: Experimental Readings for Reactor 1
No of Time (min) Conductivity (µS/cm) Concentration

obs. (M)
1 0 1550
2 3 1540
3 6 1470
4 9 1460
5 12 1460
6 15 1440
7 18 1440
8 21 1440
Table 1.8: Experimental Readings for Reactor 2
No. of Time (min) Conductivity (µS/cm) Concentration

obs. (M)
1 0 1710
2 3 1710
3 6 1560
4 9 1550
5 12 1550
6 15 1540
7 18 1540
8 21 1540
For Reactor 1
Initial Concentration of NaOH = Cao = 0.02M
Final Concentration of NaOH = Ca (final reading of concentration in first table) =
X1 = ((Cao – Ca)/Cao)*100%
For Reactor 2
Initial Concentration of NaOH = Cao = 0.02M
Final Concentration of NaOH = Ca (final reading of concentration in second table) =
X2 = ((Cao – Ca)/Cao)*100%
Total Conversion = X = X1+ X2
Post-Lab (CLO # 2)
5.6. Findings
Concentration v/s Conductivity

5000
4000 f(x) = 209187.305779988 x + 235.803682411436

R² = 0.995479156307856
Conductivity (uS/cm)
3000
2000
1000
0
0.002 0.004 0.006 0.008 0.01 0.012 0.014 0.016 0.018 0.02 0.022
Concentration of NaOH (M)
Figure 5: Effect of concentration of NaOH on conductivity

5.7. Conclusion
1. Results show that concentration of key component decreases with the increase in time
because of its consumption and product formation.
2. Results shows that Instantaneous conversion (based upon Initial Concentration) increases
with time.
3. Results shows that conductivity decreases with time as conversion increases.

• Point # 5.1 to 5.7
Experiment # 6
Experiment Title: Kinetic Studies on saponification of Ethyl Acetate.
Pre-Lab (CLO # 1)
6.1. Objective:
Obtain the reaction order by integral method of data analysis.
6.2. Process:
NaOH ( A ) +CH 3 COO C2 H 5 ( B ) →CH 3 COONa+C 2 H 5 OH

∝ β
− r A=k C A C B
Researchers typically use a batch reactor to study reaction kinetics under ideal conditions. A
batch reactor can be used to find the reaction rate constant, activation energy and order of the
reaction. The use of batch reactor for the most part eliminates the effect due to fluid flow on the
resulting reaction rates. Consequently, the data reflects the intrinsic kinetics for the reaction
being investigated.
The reaction is first order with respect to sodium hydroxide and ethyl acetate. You will
determine if your experimental data confirms the order of the reaction and the activation energy.
You will use two probes to measure the extent of reaction.
Conductivity and pH probes would be used during the experiment to determine the extent of
reaction. Conductivity probe measure the conductivity of the solution. In the present experiment,
sodium hydroxide and sodium acetate would contribute to the conductivity of the solution. Let k 0
be the conductivity of the solution at the start of the reaction. At the start, only sodium hydroxide
would contribute to the conductivity. As reaction proceeds, sodium acetate starts forming after
the consumption of sodium hydroxide resulting in different conductivity results. The
consumption of NaOH can be found using the following relationship.
C (t ) k (t ) −k ∞
=
C Ao k 0 − k ∞
Where,
C(t) = Concentration of NaOH at time t
CAo = Initial Concentration of NaOH
k(t) = Conductivity of solution at time t
k0 = Initial conductivity of solution
k∞ = Conductivity at the end of reaction
The conductivity contribution due to sodium hydroxide is different from the contribution due to
sodium acetate. So one has to find for k∞ each reaction run.
The pH probe measures the pH of the solution. The pH of the solution is directly related to the
amount of OH ions present in the solution. The formula needed to calculate the concentration of
[OH]- from pH is given below:
pH + pOH =14
≫ pOH =14 − pH
pOH =− log [OH ]−
− − pOH
[OH ] =10
For example, if pH = 12 means [OH]- = 0.01 M
Note: the value of 14 is valid only for 25oC temperature. This value changes with change in the
reaction temperature. Use the appropriate value for the experimental temperature.

the reactor system.
Time,(min) ‘κ,conductivity Concentration ‘ln(CA) ‘ln(CAo/CA) 1/CA
0
1
2
3
4
5
6
Post-Lab (CLO # 2)
6.5. Findings
6.6. Conclusion
6.7. Graph:
6
, ln(CA), 1/CA, ln(Cao/Ca)
0
0 1 2 3 4 5 6 7 8 9
Time, (min)

• Point # 6.1 to 6.7
Experiment # 7
Pre-Lab (CLO # 1)
7.1. Objective:
Plot conversion as a function of concentration of reactants and products.
7.2. Process:

∝ β
− r A=k C A C B
C (t ) k (t ) −k ∞
=
C Ao k 0 − k ∞
Where,
Conversion can be calculated as
C − CA
X = Ao
C Ao
The concentration of individual species can be calculated as
C A=C Ao ( 1 − X )
b
C B=C Ao (ƟB − X)
a
c
C C =C Ao(ƟC + X )
a
d
C D =C Ao (Ɵ D + X )
a

the reactor system.
Time,(min) ‘κ,conductivity Concentration X CA CB CC CD
0
1
2
3
4
5
6
7
Post-Lab (CLO # 2)
7.5. Findings
7.6. Conclusion
7.7. Graph:
X vs. CA, CB, CC, CD

12
10
CA, CB, CC, CD 8
0
0 2 4 6 8 10 12
Conversion, X

• Point # 7.1 to 7.7
Experiment # 8
Pre-Lab (CLO # 1)
8.1. Objective:
Determine the specific reaction rate constant.
8.2. Process:

∝ β
− r A=k C A C B
C (t ) k (t ) −k ∞
=
C Ao k 0 − k ∞
Where,
Rate constant can be calculated as
Ao
2.303 log =kt
At
Ao k
log = t
A t 2.303
The equation looks like y = mx+c
Plot log (Ao/At) vs. time to find the slope of the graph, which is the rate constant for the
reaction.

the reactor system.
time conductiv concentrati ‘log(Cao/

ity on Ca)
0
1
2
3
4
5
6
7
8
Post-Lab (CLO # 2)
5.5. Findings
8.6. Conclusion
8.7. Graph:
5
, log(Cao/Ca) 4
0
0 1 2 3 4 5 6 7 8 9
Time, (min)

• Point # 8.1 to 8.7
Experiment # 9
Experiment Title: Demonstrate that the saponification of the ethyl-acetate with sodium
hydroxide is a reaction of first order with respect to ethyl-acetate.
Pre-Lab (CLO # 1)
9.1 Objective
Demonstrate that the saponification of the ethyl-acetate with sodium hydroxide is a

reaction of first order with respect to ethyl-acetate, using the initial velocity method described in
Section 7.2.2.2.
9.2 Chemicals:
● 10 L of ethyl-acetate (0.1 M solution)

● 10 L of Sodium Hydroxide (0.05 M solution)
● QRSC System
9.3 Process:
Due to the method employed to obtain the velocity equation, some calculations should be
performed in advance. First, from the ethyl-acetate 0.1 M solution, new concentrations will be
obtained by dissolution
Each reactant deposit will be loaded with 10 litres of reactant solution, while the Sodium
Hydroxide concentration will be kept constant, the concentration of ethyl-acetate will be
changed in each experiment.
Once the first experiment has been carried out, add 1 litre of water to the deposit with the
ethyl-acetate. The concentration now will be
N initial V initial=N final V final [3.5.1]
where N (initial) and N (final) are the initial and final normalities of the solution
respectively, and V (initial) and V (final) are the initial and final volume of the solution
respectively.
In this case, because of the reactant used the normality and molarity are equivalent.
For the first dissolution:
}
N initial=5 N
V initial=91
→ N final = 5 N × 91 =4.5
N final 101
V final=101
Compute the different concentrations of the ethyl-acetate dissolutions, filling the table below:
Experiment Initial concentration Concentration used C A 0

1 0.1M 0.1M
2 0.1M 0.09M
3 0.09M
4
5
Concentrations of ethyl-acetate used in the different experiments
9.4 Experimental Procedure:
Now the different concentrations have been computed, the experiments can be performed.
1. Start the SACED-QUSC software
2. Press Start and input the data filename
3. Put the corresponding reactants in the deposits of the QRCAC unit
4. Recirculate water until a constant flow is obtained
5. Start the thermal system and set the desired working temperature to 25℃
6. Open sodium hydroxide valve to the “To Reactor” position and allow 1 litre of the
solution to the reactor, turn the valve to the “Recirculation” position.
7. Start the stirrer to help in thermal homogenisation, wait until the temperature is stable
around 25℃
8. Measure the conductivity of the ethyl-acetate solution
9. Open the ethyl-acetate valve to the “To Reactor” position and allow 1-litre o solution into
the reactor. Return the valve to the “Recirculation” position.
10. Once the conductivity is table the reaction is finished.
11. Stop the stirrer
12. Empty the reactor through the “Product Output 1” valve.
13. Fill the table with the obtained data
14. Add 1 litre of water to the ethyl-acetate reactant deposit
15. Repeat points 1 through 16 for four different concentrations.
16. Stop the feed system
17. Turn the three-way valves to the “Close” position
18. Turn off the stirrer.
19. Turn off the thermal bath heating element
20. Empty the product deposit.

With the data obtained in each of the reactions, complete the following tables using the formula
below and the value of ionic conductivity difference obtained in previous practice.
( K − K t =t ). 103
C A= t=0 [3.6.2]
λoℎ − λ R
− −
Plot theC etℎyl − acetate vrs. time

Initial concentration of ethyl-acetate: M
Time(min) Conductivity C ethyl −acetate
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
Ethyl-acetate concentration ____M
For the previous plots draw the tangent to the curve (t,C etℎyl − acetate ),at t=0 and find the initial
velocity for each of the concentrations. Fill the table below
Concentration r0
=C 0.1 =r 0.1
=C 0.2 =r 0.2
=C 0.3 =r 0.3
=C 0.4 =r 0.4
=C 0.5 =r 0.5
Initial velocities for the different concentrations of ethyl-acetate.
The ratio of velocity and initial concentration will give this reaction order respect to ethyl-
acetate.
α
r 0.1 C 0.1
=( ) [3.5.3]
r 0.2 C 0.2
Using the data from the previous table, complete the following:
r 0.1 /r 0.1 +t C 0.1/C 0.1+t α
Thus the order of the reaction with respect to ethyl-acetate is
α=
Post-Lab (CLO # 2)
9.6 Findings
9.7 Graph:
Time evolution of the ethyl-acetate concentration.

Point *9.1 to 9.7
Experiment # 10
Experiment Title: Demonstrate the dependency of the velocity constant with
temperature obeying the law of Arrhenius constant.
Pre Lab(CLO1)
10.1 Objective
Demonstrate the dependency of the velocity constant with temperature obeying the law
of Arrhenius:
− Ea
RT
K= A e
where A and E, are constants of the reaction and R is the gas constant. E is known as the
Arrhenius activation energy and A is the pre-exponential factor or Arrhenius factor-A.
10.2 Chemicals:
● 10 litres of ethyl acetate solution 0.1 M

● 10 litres of sodium hydroxide solution 0.1 M
● QRSC unit

1. Start the SACED-QUSC software
2. Press the START button and input the file name to save the data.
3. Place enough ethyl-acetate solution in the reactor to cover the conductivity cell and
thermocouple.
4. Start the thermal bath and set 25°C as working temperature.
5. Start the stirrer to help homogenise the temperature.
6. Determine the conductivity of ethyl-acetate at 25°C.
7. Add 1 litre of sodium hydroxide solution.
8. Measure for 30 minutes.
9. Repeat the measurements for 35 and 45°C.
10. Log the results in table 3.11.1,
11. Empty the reactor
12. Clean with water and rinse several times.
Fill the following tables with the values obtained in the previous practices and the
C A 0 −C A
graphical representation of ln find the velocity constant values for the different
CH 0− CA
temperatures.
Complete with the obtained values, the following table.
Temperature:C°
Time(min) C A 0 −C A
ln
CH 0− CA
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
Needed computation to find the the velocity constant at C° .

C A 0 −C A
Graphical representation of ln vs. Time for a temperature of C° .
CH 0− CA
Complete , with the obtained values, the following table:
Experimen Temperature C A0 CB0 CA 0 C A 0 −C B 0 K

ln
t (C° ) (M) (M) CB0
Summary of the values obtained in the experiments performed, where C A 0 is the initial
concentrations of ethyle-acetate and C B 0 the initial concentration of sodium hydroxide.
Computing the log of the equation [3.11.1] we have
Ea
lnK =lnA −
RT
Ea
logK =logA −
2.0303 RT
[3.11.2]
If the Arrhenius equation is met, a plot of log k vs IT should give a
straight line with a slope - E_{2} / 2.0303 * F and intercept logA
Plot the values of log k vs. 1/T and perform a least-square fit to obtain the value of A * Anhenius
factor and the Activation Energy, E_{3}
The values obtained are:
− Ea Ea logA A
2.0303 R
Regression for logK vs. 1/T.
10.5. Graph:
Graphical representation of logK vs. 1/T.

Post-Lab (CLO # 2)
10.6 Conclusions and comments

● What are the units for the Arrhenius factor?
● What is the reason for the presence of that factor in the Arrhenius equation?
● What are the units of the activation energy?
● What does high activation energy mean?
● And low activation energy?

• Point # 10.1 to 10.6
Experiment # 11
Experiment Title: experimental determination of tubular reactor conversion.
Pre Lab(CLO1)
11.1 Objective
Determine experimentally the tubular reactor conversion.
11.2 Chemicals:
● QRC unit.
● 1 litre of dissolution 0.1 M of NaOH.
● 1 litre of dissolution 0.1 M of ethyl-acetate.

1. Fill a tank with 1 1 of the ethyl acetate dissolution and another tank with 11 of the NaOH
dissolution.
2. Switch on the interface. Start the QRC software,
3. A welcome window appears. Select the reactor understudy, QRTC in this case.
4. Press the START button and introduce in the new window the file name which will have
the data.
5. Put a set point in the program the temperature at which you want to work (e. g. 30° C).
6. Put the same flow in both pumps and start them from the program.
7. Measure the conductivity values during all the processes. When the conductivity cell
marks a constant value (the process has been stabilized), write down the obtained result.

With the value obtained in the practice 2 and carrying out the calculations of section
7.2.5.1, calculate the NaOH concentration at the reactor outlet.
 Calculate the conversion factor.
Concentration of NaOH in the reactor flow:
Q A C AT
At the inlet : C A 0= (the present one in the reactive tank)
Q A +Q B
Q A C As
At the outlet: C Ai=
Q A +QB
Conversion at outlet:
C Ai − C A 0
X=
C Ai
Post-Lab (CLO # 2)
11.5. Findings
Comment the obtained results, comparing them with the obtained ones in the previous
practice.

• Point # 11.1. to 11.5.
Experiment # 12
Experiment Title: Dependence on the residence time
Pre Lab(CLO1)
12.1 Objective
Determine the conversion regarding the residence time.
12.2 Chemicals:
● QRC unit.
● Analytic unit of the practice 1.
● 1 litre of dissolution 0.1 M of ethyl acetate.
12.3 Experimental procedure:
1. Fill a tank with II of the ethyl acetate dissolution and another tank with 1 litre of the
NaOH dissolution.
2. Switch on the interface. Start the QRC software.
3. A welcome window appears. Select the reactor under study. QRTC in this case.
the data
5. Set the temperature at which you want to work (e.g 30°C) in the program, which must be
constant during all the practice
6. Select an initial flow in the low range of the pumps, so that both flows are the same, it is
to say, that the reaction is mole by mole.
7. When the conductivity cell marks a constant value (the process has been stabilized), write
down the obtained result.
8. Stop the pumps and mark in them a different flow value. Repeat the measurement for
different values of Q, y On
Write down the obtained values in the following table.
Conc. In the Flow(1/s) Total flow θ=V /Q C A X X

tank(mole/1) (1/s) measured 1− X
C NAOH C AeoH Q NaOH Q AeOH Q=Q1 +Q 2
C NAOH . Q NaOH
Values obtained in the practice , C A=
Q
To obtain the volume, recall that the reactor length is 20 metres and its internal diameter is 6
metres.
Post-Lab (CLO # 2)
12.5. Findings
Represent θ to X (for a good adjust, minimum four points).
Comment on the obtained graph

Representation of the time regarding to the conversion factor.
• Point # 12.1. to 12.5.
Experiment # 13
Experiment Title: Determination of the reaction order
Pre Lab(CLO1)
13.1 Objective
Determination of the reaction order and the speed constant.
13.2 Chemicals:
● QRC unit.
● Analytic unit of the practice 1.
● 1 litre of dissolution 0.1 M of ethyl acetate
13.3 Experimental procedure:
1. Fill a tank with II of the ethyl acetate dissolution and another tank with 11 of the NaOH
dissolution..
2. Switch on the interface. Start the ORC software.
3. A welcome window appears. Select the reactor understudy, QRTC in this case.
the data.
5. Set the temperature at which you want to work (e.g 30°C) in the program, which must be
constant during all the practice.
6. Select an initial flow in the low range of the pumps, so that both flows are the same, it is
to say, that the reaction is mole by mole.
7. When the conductivity cell marks a constant value (the process has been stabilized) write
down the obtained result.
8. Stop the pumps and mark in them a different flow value.
9. Repeat the measurement for different values of Q Non and Quo (Q R =Q A * C A C
mu ), Try to carry out more than 4 experiences, in order to be able to do a good enough
analysis of the results.
Conc. In the Flow(1/s) Total flow θ=V /Q C A X X

tank(mole/1) (1/s) measured 1− X
C NAOH C AeoH Q NaOH Q AeOH Q=Q1 +Q 2
C NAOH . Q NaOH
Values obtained in the practice , C A=
Q
Represent θ face LnC A and θ face to 1/C A.
Take into the account that, if the reaction order 1, the representation of the θ face to LnC A will give a
straight line; while if the reaction is of order 2, the representation of θ face to 1/C A will be a straight
line.
From a suitable graph slope, determine K.
Note: if the θ is in seconds and C A. in mole/1, K will have units of liters/moles.

Post-Lab (CLO # 2)
13.5. Findings
Representation of the time regarding to the concentration logarithm.
Representation of the time regarding to the concentration inverse.

• Point # 13.1. to 13.5.

CRE Manual

Uploaded by

Copyright:

Available Formats

CRE Manual

Uploaded by

Document Information

Original Description:

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

CRE Manual

Uploaded by

Copyright:

Available Formats

LIST OF EXPERIEMNTS IN CHEMICAL RREACTION ENGINEERING (LAB)

1. Analyze the effect of concentration on the rate of a chemical reaction

1. Describe the fundamentals of Chemical Reaction Engineering lab experiments and

3. Perform all experiments by following standard operating procedure (SOP) and

6. Commit to basic human or professional ethics and teamwork attributes

PROGRAMME LEARNING OUTCOMES (PLOs)

Safety Rules and Regulations

1. Have I done this before?

2. Do I have the proper equipment?

3. Does anything look wrong?

4. What are the hazards?

5. Should I work in a fume hood?

6. Do I need goggles or other safety equipment?

7. Do I need additional help?

8. Should I check further with my instructor?

9. Have I planned this experiment or exercise?

10. Do I know what to do, if there is an accident?

11. Do I know where the fire extinguishers are located?

1. NO SMOKING IS ALLOWED IN THE LABORATORY PREMISES.

4. Wear rubber gloves when handling liquids.

6. Find out the location of First Aid Box.

13. Avoid inhalation of gases or vapors of any kind.

16. Make sure any system being heated is properly vented.

18. Do not smell directly any chemical being heated.

24. All power wiring is to be installed by an approved electrician.

25. Always remember: SAFETY IS GOOD TECHNIQUE!

Analyze the effect of concentration on the rate of a chemical reaction

Na2S2O3 + 2HCl → 2 NaCl + H2O + S + SO2

0.15 M sodium thiosulfate solution

25-mL graduated cylinder

In-Lab (CLO # 3, CLO # 5, CLO # 6)

1.7 Safety Observations:

1.8 Observations and Calculations:

Figure 1: Effect of concentration on rate of chemical reaction

Organization of lab reports

Analyze the effect of concentration on the rate of a chemical reaction

Na2S2O3 + 2HCl → 2 NaCl + H2O + S + SO2

0.15 M sodium thiosulfate solution

25-mL graduated cylinder

In-Lab (CLO # 3, CLO # 5, CLO # 6)

2.7 Safety Observations:

2.8 Observations and Calculations:

Na2S2O3 distille Concentration disappearance (1/time, sec-1)

Figure 2:Effect of concentration on rate of chemical reaction

Organization of lab reports

Analyze the effect of surface area (particle size of a solid reactant) on

CaCO3(s) + 2HCl(aq) → CaCl2(aq) + CO2(g) + H2O(l)

1. 1 Set up the apparatus as shown in the diagram.

In-Lab (CLO # 3, CLO # 5, CLO # 6)

3.4. Safety Observations:

5. Drain the reactors carefully.

Time (sec) Volume of Co2 (ml), Vt Vf-Vt (ml)

Experiment Title: Batch Reactor

Measure the conversion of saponification reaction in Batch reactor

4.2. Process and Applications:

CH3COOC2H5+ NaOH →CH3COONa + C2H5OH

The conversion of sodium hydroxide is calculated as:

X NaOH = ((CNaOH,o − CNaOH)/ CNaOH,o)*100%

4.3. Experimental Procedure: