CRE Lab Manual

Laboratory Manual
CHEMICAL REACTION ENGINEERING CHE-324
Department of Chemical Engineering

COMSATS Institute of Information & Technology, Lahore, Pakistan.
Prepared By:
Engr. Hasan Qayyum (Lab Engineer)
Engr. Fawad Ashraf (Lab Engineer)
Laboratory Handbook
1. Course Title Chemical Reaction Engineering Laboratory
2. Course Code CHE-324
3. Credit Hours 4(3,1)
4. Semester 6th
5. Resource Person Engr. Hasan Qayyum (Lab In-charge)
6. Supporting Team Members Fawad Ashraf (Lab Engineer)
7. Contact Hours (Lab) 1
8. Lab Introduction
Chemical Reaction Engineering laboratory practice is the core curriculum in the specialties of Chemical
Engineering and Technology. Through conduction of laboratory experiments during the CRE-Lab, students will
support their theoretical knowledge of industrial reactors. The laboratory practice aims at strengthen student
knowledge of developing stoichiometric table for reactions, collection and analysis of rate data, evaluation of
kinetic parameters and developing of rate equations. Furthermore, student will perform experiments on Batch,
CSTR, CSTR’s in series and tubular reactors.
9. Learning Objectives
The objectives are to study the kinetics of chemical reaction carried out in laboratory reactors. The following are
the partial objectives that you are expected to master by the end of this laboratory practice.
Development of stoichiometric table for reactions.
Using kinetic data from batch reactor experiments to scale up liquid phase batch reactor.
Using numerical techniques to find the order and specific reaction rate constant.
Study the effect of concentration and temperature on the rate of reaction.
Investigate the molar flow rates of reagents entering the reactor.
Determine the time necessary to achieve a certain conversion in a batch reactor.
Plotting experimental data to study the conversion down the length of a reactor.
Investigate the temperature dependency of rate constant.
Calculating the residence time reactant spent in the reactor.
Evaluation of reactors for different operating conditions.
Finding the maximum conversion that could be achieved in the CSTR’s connected in series.
10. Lab Contents
Investigating the effect of concentration and temperature on rate of chemical reaction.
Studying the temperature dependence on specific reaction rate constant.
Kinetics study on batch reactor.
Time to achieve certain conversion in a batch reactor.
Determination of order and rate constant for saponification reaction.
Calculating the theoretical conversion achieved in a tubular reactor.
Determine the activation energy of the chemical reaction.
Comparing the conversion for single CSTR and CSTR’s in series.
Investigating the reagent residence time / Space time.
11. Laboratory Exercise Plan
Reading
Weeks List of Experiments Assignment
Week 1 Introduction to Chemical Reaction Engineering-Laboratory/ Learning Industrial
Objectives/ Laboratory Equipment/ Lab hand-book introduction. Reactors.
Week 2 Experiment-1
Investigating the effect of concentration on the rate of a chemical reaction.
Week 3 Experiment-2
Investigating the effect of Temperature on the Rate of a Chemical Reaction.
Week 4 Experiment-3
Investigating the effect of surface area (particle size of a solid reactant) on the
rate of a chemical reaction.
Week 5 Quiz-1/ Assigment-1
Week 6 Experiment-4
Investigate the molar flow rates of reagents entering the chemical reactors by
calibrating the peristaltic pump.
Week 7 Sessional-1 Exam
Week 8 Experiment-5 (EDIBON Training Panel) Collection &
Determination of final conversion achieved through tubular reactor. Analysis of Rate
Data.
Week 9 Experiment-6 (EDIBON Training Panel)
Prove that dCA/dt is not the rate of reaction for tubular reactor.
Week 10 Experiment-7 To carry out saponification of ethyl acetate in three CSTR’s in

series and to determine the conversion and to compare with single CSTR.

Kinetic Studies on saponification of Ethyl Acetate.
Plot conversion as a function of concentration of reactants and products
Week 12 Sessional-2 Exam
Obtain the reaction order by integral method of data analysis.
Determine the specific reaction rate constant.
Prove that dCA/dt is rate of reaction for batch reactor.
Week 16 Review of lab experiments/ Instruction for laboratory reports/ Quiz and
Assignment solutions.
Final Examination.
12. Laboratory Assessment
The assessment of this module shall have following breakdown structure
First Sessional Test 10%

Second Sessional Test 15%
Quizzes/Assignments 25%
Terminal Examination 50%
The minimum pass marks for each course shall be 50%. Students obtaining less than 50% marks in any course
shall be deemed to have failed in that course. The correspondence between letter grades, credit points, and
percentage marks at CIIT shall be as follows:
Grades Letter Credit Points Percentage Marks
Grade
A ( Excellent) 4.0 90and above
A- 3.7 85-89
B+ 3.3 80-84
B (Good) 3.0 75-79
B- 2.7 70-74
C+ 2.3 65-69
C (Average) 2.0 60-64
C- 1.7 55-59
D (Minimum 1.3 50-54
passing)
F (Failing) 0.0 Less than 50
Note: The marks to be assigned to students shall be in whole numbers and are not same as followed in the annual
system of Lancaster University.
13. Assessment Schedule
Week 2 Assignment-I
Week 4 Quiz-I
Week 6 Sessional-I
Week 7 Assignment-II
Week 10 Quiz-II
Week 12 Sessional-II
Week 14 Assignment-III
Week 16 Quiz-III
Weeks 18-19 Terminal Examination
14. Format of Assignment

This course indoctrinates the following format for all its assignments:
1. Paper Size: A4
2. Left Margin: 2 Inches
3. Right Margin: 1 Inch
4. Top Margin: 0.5 Inch
5. Bottom Margin: 0.5 Inch
6. Font: Times New Roman
7. Font Size:
a. Main Heading 14
b. Sub Heading 12
c. Text 12
d. Titles 16
8. Font Color: Black
9. Line Spacing: 1.5
10. Diagrams & Charts: Need not be colored
11. Title page must be designed as guided by resource person in class
12. Number of Pages: No Limit
Reference Style: APA (If applicable)
15. Text Book
Fogler, H. Scott, “Elements of Chemical Reaction Engineering 4th Edition” ISBN 10: 0130473944 / 0-13-
047394-4, Publisher: Prentice Hall (2008).
16. Reference Book
1). “Chemical Engineering kinetics”, (Smith J.M., McGraw Hill Book Co., 3rd Ed. 2001).
2). “Chemical Reactor Engineering”, (Levenspiel Octave., John Willey & Sons Inc., 2nd Ed. 1999
3). “Chemical Reactor Design, Optimization and Scale up”, (E. Bruce Naumen McGraw Hill 2002).
17. Plagiarism
Plagiarism involves the unacknowledged use of someone else’s work, usually in coursework, and passing it off
as if it were one’s own. Many students who submit apparently plagiarized work probably do so inadvertently
without realizing it because of poorly developed study skills, including note taking, referencing and citations;
this is poor academic practice rather than malpractice. Some students, particularly those from different cultures
and educational systems, find UK academic referencing/acknowledgement systems and conventions awkward,
and proof-reading is not always easy for dyslexic students and some visually-impaired students. Study skills
education within programmes of study should minimize the number of students submitting poorly referenced
work. However, some students plagiarize deliberately, with the intent to deceive. This intentional malpractice is
a conscious, pre-mediated form of cheating and is regarded as a particularly serious breach of the core values of
academic integrity.
The Dual Degree Programme has zero tolerance for intentional plagiarism.
Plagiarism can include the following:
1. collusion, where a piece of work prepared by a group is represented as if it were the student’s own;
2. commission or use of work by the student which is not his/her own and representing it as if it were, e.g.:
a. purchase of a paper from a commercial service, including internet sites, whether pre-written or
specially prepared for the student concerned
b. submission of a paper written by another person, either by a fellow student or a person who is not a
member of the university;
3. duplication (of one’s own work) of the same or almost identical work for more than one module;
4. the act of copying or paraphrasing a paper from a source text, whether in manuscript, printed or electronic
form, without appropriate acknowledgement (this includes quoting directly from another source with a
reference but without quotation marks);
5. submission of another student’s work, whether with or without that student’s knowledge or consent;
6. Directly quoting from model solutions/answers made available in previous years;
7. cheating in class tests, e.g.
a. when a candidate communicates, or attempts to communicate, with a fellow candidate or individual
who is neither an invigilator or member of staff
b. copies, or attempts to copy from a fellow candidate
c. attempts to introduce or consult during the examination any unauthorised printed or written material,
or electronic calculating, information storage device, mobile phones or other communication device
d. Personates or allows himself or herself to be impersonated.
8. Fabrication of results occurs when a student claims to have carried out tests, experiments or observations
that have not taken place or presents results not supported by the evidence with the object of obtaining an
unfair advantage.
These definitions apply to work in whatever format it is presented, including written work, online submissions,
group work and oral presentations.
18. Attendance Policy
Every student must attend 80% of the lectures/seminars delivered in this course and 80% of the
practical/laboratory work prescribed for the respective courses. The students falling short of required percentage
of attendance of lectures/seminars/practical/laboratory work, etc., shall not be allowed to appear in the terminal
examination of this course and shall be treated as having failed this course.
19. Instruction for preparing laboratory report
1. Title Page
The Title page should be separate from the rest of the report. It should contain:
a. The title of the experiment.
b. The number of course.
c. The names of the writer and his co-worker(s), their ID numbers, and group number.
d. Name of the instructor to whom the report is submitted
e. The date when the experiment was run
f. The date of submission of report.
2. Abstract
The abstract should be informative, and should be written in about three to five sentences. It should cover all
phases of the investigation. It must include the following:
a. An introductory statement about the subject matter
b. Brief description of what was done and how it was done.
c. Selected results (numerical values, if available).
d. Brief assessment of the results e.g. some percentage errors in
Experimental results in comparison with theoretical values.
While writing the abstract, no reference should be made to graphs, tables or equations inside the report.
3. Introduction
This section should include few sentences discussing the physical and/or chemical principles involved in the
experiment. The importance and relevance of the experiment to real applications may also be stated.
4. Theoretical Background
This section should include the theory behind the experiment. It should also contain all those equations, which
are used to acquire a certain result. Theoretical correlations, which are used for comparison with experimental
results, should also be included.
5. Procedure
Here, you should briefly describe the actual step-by-step procedure you followed in running the experiment. It
should be written in your own words, e.g. the needle valve was manipulated in order to adjust the liquid flow
rate.
6. Results
The results should be presented in the form or Tables or graphs. The Table should contain the results obtained
from experiments and from theoretical knowledge.
Comparisons may also be presented in terms of percent deviation between experimental values and theoretical
predictions.
7. Discussion of Results
In this section you should discuss your experimental results and observations. If the results are obtained in terms
of graphs, then interpret them also. Describe observed trends and possible relationship between parameters e.g.
how a change in one variable affects another. Also show how you make comparison with the values obtained
theoretically and discuss the deviation of experimental results from theoretical values. The possible source of
errors should also be mentioned.
8. Conclusions and Recommendations
Conclusions are the series of numbered sentences which answer the questions posed at the beginning of each
experiments. Conclusions should also include main results (numerical values) and the errors between the
experimental and theoretical values. What you have learned from the experiment should be mentioned as well.
Recommendations are the proposals for future work, e.g. suggested changes in equipment, Study of new
variables, or possible experiments in relative fields. Like the conclusions, the recommendations are usually listed
by numbers, and each consists of only a sentence or two.
9. Literature Cited
Here, you should list the books, Journal’s articles, etc. used in writing your report and analyzing the experiment.
The reference should be completed (name of the book, author, volume, date of publication, pages, etc.).
References should be arranged alphabetically by author’s names.
10. Nomenclature
The symbols, which are used in the report, should be defined in the nomenclature in alphabetical order. The
accompanying definitions must include proper units.
Appendices
All appendices and graphs should be attached at the end of the report.
20. Safety Rules and Regulation.
DOs and DON’T DOs in Laboratory:
1. Do not enter the laboratory without wearing apron, preferably use shoes.
2. Safety should be given topmost priority.
3. Follow the instructions given by the teacher.
4. Do not touch any Equipment/Chemicals without prior permission.
5. Check the glassware before getting issued.
6. Handle the chemicals carefully as per instructions.
7. Do not pipette any solution/chemical with mouth.
8. During performance of the practical if any glassware is broken inform immediately.
9. Return the borrowed apparatus after the experiment is over.
10. Observe safety precautions while performing the experiment.
Instruction for Laboratory Teachers:

1. Submission related to lab work should be completed before the next lab session.
2. The promptness of submission should be encouraged by way of marking and evaluation patterns that will
benefit the sincere students.
Introduction:-
The laboratory of Chemical Reaction Engineering is designed for undergraduate students to broaden their
theoretical knowledge of industrial reactors. Students will perform kinetics experiments on lab scale industrial
reactors to evaluate rate data. Following reactors are in the CRE-lab for conducting experiments:
Batch Reactor:-
Batch reactors are perhaps the simplest reactors used in chemical processes. When using batch reactors, reactants
are first placed inside the reactor and then allowed to react over time. Batch reactors are closed systems that
operate under unsteady-state conditions. The reactors shown below is laboratory scale batch reactor.
Figure 1 Laboratory Batch Reactor (EDIBON, Spain)
While batch reactors are used in a variety of situations, they have some common design features.
Batch reactors contain ports for injecting reactants and removing products, and can be outfitted with a heat
exchanger or a stirring system. While batch reactors are generally of constant volume, some are designed to
maintain a constant pressure by varying the reactor volume.
Batch reactors are used in a wide variety of applications. Typically, they are used for liquid phase reactions that
require a fairly long reaction time. Batch reactors are also used when only a small amount of product is desired.
For this reason batch reactors are favored when a process is still in the testing phase, or when the desired product
is expensive. Batch reactors, like the one below, are used in the pharmaceutical industry, which requires
consistent, high quality results. One batch reactor may also be used to make a variety of products at different
times.
ADVANTAGES DISADVANTAGES
 High conversions can be obtained by leaving  High cost of labor per unit of production.
reactants in reactor for extended periods of  Difficult to maintain large scale production.
time.  Long downtime for cleaning leads to periods
 Batch reactor jackets allow the system to of no production.
change heating or cooling power at constant
jacket heat flux.
 Versatile, can be used to make many
products consecutively.
 Good for producing small amounts of
products while still in testing phase.
 Easy to clean.
Continuous Stirred Tank Reactor:-
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 immicible
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. Fermentors are CSTRs used in biological processes in many industries, such as brewing,
antibiotics, and waste treatment. In fermentors, large molecules are broken down into smaller molecules, with
alcohol produced as a by-product. Pictured below is the CSTR placed in the laboratory of CRE.
Figure 2 Continuous Stirred Tank Reactor (EDIBON, Spain)

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.
 Good temperature control is easily  Conversion of reactant to product per
maintained volume of reactor is small compared to other
 Cheap to construct flow reactors
 Reactor has large heat capacity
 Interior of reactor is easily accessed
Continuous Stirred Tank Reactor in Series:-
Sometime reactors are connected in series to study the final conversion that could be achieved. In this laboratory
students are expected to learn conversion achieve in a single CSTR and compare it with conversion achieved in
the CSTR’s connected in series.
Figure 3 CSTR's connected in series (EDIBON, Spain).
Plug Flow Reactor:-

Plug flow, or tubular, reactors consist of a hollow pipe or tube through which reactants flow. Pictured below is
a plug flow reactor in the form of a tube wrapped around an acrylic mold which is encased in a tank. Water at a
controlled temperature is circulated through the tank to maintain constant reactant temperature. Plug flow
reactors, also known as tubular reactors, consist of a cylindrical pipe with openings on each end for reactants and
products to flow through. Plug flow reactors are usually operated at steady-state. Reactants are continually
consumed as they flow down the length of the reactor. Plugs of reactants are continuously fed into the reactor
from the left. As the plug flows down the reactor the reaction takes place, resulting in an axial concentration
gradient. Products and unreacted reactants flow out of the reactor continuously. Plug flow reactors have a wide
variety of applications in either gas or liquid phase systems. Common industrial uses of tubular reactors are in
gasoline production, oil cracking, synthesis of ammonia from its elements, and the oxidation of sulfur dioxide to
sulfur trioxide. Pictured below is a tubular reactor placed in the laboratory of CRE.
Figure 4 Plug flow reactor (EDIBON, Spain).
 Easily maintained since there are no moving  Reactor temperature difficult to control.
parts.  Hot spots may occur within reactor when
 High conversion rate per reactor volume. used for exothermic reactions.
 Mechanically simple.  Difficult to control due to temperature and
 Unvarying product quality. composition variations.
 Good for studying rapid reactions.
 Efficient use of reactor volume.
 Good for large capacity processes.
 Low pressure drops.
Experiment 1:
Investigating the effect of concentration on the rate of a chemical reaction.
Objective: To investigate the concentration and temperature effects on the rate of a chemical reaction
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.
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.
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.
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
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:
Beakers Vol. of Na2S2O3 Vol. of Volume and Time until cross disappearance.
distilled Concentration of
solution (ml)
water sodium 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)
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.
DISPOSAL
Small amounts of colloidal suspensions of sulfur can be washed down the drain.
Data Analysis
1. Calculate the initial concentration of sodium thiosulphate in the reaction mixtures.
2. Plot the time required for the disappearance of the cross against the initial concentration of sodium
thiosulphate on a graph paper. Label your graph properly.
3. How is the rate of reaction affected by the concentration of the reactant?
Experiment-2
Investigating the effect of temperature on the rate of a chemical reaction.
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
o
Temperature: 25-30 C (refer to data taken in experiment-1)
Room temperature (refer to the data taken in Exp-1)
50-70oC (by warming the Na2S2O3 solution with a 50-70oC water bath)
Procedure Reaction at 25-30oC
Same as in experiment -1, for higher temperature heat the solution up to 50-60C in water bath.
Results: -
Time for the disappearance of the cross
Vol. of Vol. of Volume and Time until cross Reaction Rate
Na2S2O3 distilled Concentration disappearance
(1/time, sec-1)
water of sodium
Beakers
solution (sec)
thiosulfate
(ml)
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)
Graph (Expected)
60
50
Time, (sec)
40
30
35C
20
60C
10
0
0 0.02 0.04 0.06
Concentration, (M)
Data Analysis
1. From the data in the above table, how is the rate of reaction affected by temperature?
Experiment 3:
Investigating the effect of particle size of a solid reactant on the rate of a
chemical reaction.
Objective: To investigate the effect of surface area on the rate of a chemical reaction
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.
1. 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.
2. 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)
3. 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.
4. Wear eye protection
5. Take care with the gas syringe
6. 1 Set up the apparatus as shown in the diagram.
7. 2 Place about 10 g of marble in six or seven lumps in the test tube.
8. 3 Use a measuring cylinder to measure 10 cm3 of 1 M hydrochloric acid.
9. 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.
10. 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.
11. 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.
12. 7 Plot a graph of (Vfinal – Vt) against t, putting t on the horizontal axis.
13. Record your results in a table like the one below.
Time (sec) Volume of Co2 (ml), Vt Vf-Vt (ml)
Experiment 4: Determination of rate parameters for a chemical reaction
Objective: To determine the rate equation for the reaction of iodine and propanone in acidic medium
Introduction:
From experiment 1 you should have realized that the rate of a chemical equation depends on its reactants’
concentration. The relationship between the rate of a chemical reaction and its reactants’ concentration can be
expressed into a rate equation. For example, propanone reacts with iodine in acidic medium as shown below:
CH3COOCH3(aq) + I2(aq)  CH3COCH2I(aq) + H+(aq) + I-(aq)
The rate of the reaction may depend on the concentration of propanone (CH3COCH3), iodine (I2) and
acid (H+). The rate equation of the reaction can be expressed in the form of:
Rate = k[CH3COCH3]a[I2]b[H+]c
Where [CH3COCH3], [I2] and [H+] are the concentration of propanone, iodine and acid, respectively.
k is the rate constant which is a quantity that depends on reaction temperature. a, b and c are the orders of reaction
with respect to propanone, iodine and acid, respectively. Reaction orders (a, b and c) are quantities that must be
determined experimentally and cannot be deduced from the chemical equation. The reaction order with respect
to a reactant is not necessarily equal to the reactant’s coefficient present in the balanced chemical equation.
In this experiment you are going to determine the values of k, a, b, and c for the reaction of propanone
with iodine. You will do so by running the reaction several times and varying the concentration of the reactants
one at a time.
Chemicals: 1 M hydrochloric acid

1 M propanone
0.002 M iodine solution (prepared by dissolving 0.5 g of I2 and 3.3 g of KI in 1 L of deionized
water)
Apparatus: measuring cylinders, conical flasks
Procedure:
1. Use measuring cylinders to measure the appropriate amounts of hydrochloric acid, propanone solution and
deionized water into dry conical flasks, according to the table shown below.
2. Add appropriate amounts of iodine solution into the conical flasks. Start the stop watch.
3. Swirl the flasks gently.
4. Measure the time taken for the colour of iodine disappears completely.
Data:
Run 1 Run 2 Run 3 Run 4
Volume of 1 M HCl(aq) (mL) 20 10 20 20
Volume of 1 M CH3COCH3(aq) (mL) 8 8 4 8
Volume of deionised water (mL) 0 10 4 2
Volume of 0.002M I2(aq) (mL) 4 4 4 2
[I2] in the time taken (mol dm-3)

Time for the disappearance of the Trial 1
colour (s)
Trial 2
Average
Initial rate of reaction (mol dm-3 s-1)
Data Analysis:
1. Calculate the initial concentration of I2 in the reaction mixture and hence the change in iodine
concentration in the time taken.
Run 1
Run 2
Run 3
Run 4
2. Calculate the rate of consumption of I2, this is the initial rate of reaction in terms of I2.
Run 1
Run 2
Run 3
Run 4
3. Determine the order of reaction with respect to each reactant.
4. Estimate the rate constant (with unit) for the reaction using the data in Run 1.
5. Write the rate equation for the reaction.

Experiment 5: To estimate nature of temperature dependency of rate
constant of in dilute aqueous solution.
Objective: To estimate nature of temperature dependency of rate constant of ethyl acetate with NaOH in dilute
aqueous solution.
Chemicals Required: Ethyl acetate =0.1 N, Hcl, NaOH= 0.1 N, Std. Oxalic acid, phenolphthalein indicator,
pipette, burette etc.
Procedure:
1) Adjust the thermostat to obtain the constant temperature.
2) Take 25 ml of ethyl acetate solution in one standard flask of 100 ml and mount it in the thermostat (flask 1)
3) Take 25 ml of 0.1 N NaOH solution in one standard flask of 100 ml and mount it in the thermostat (flask 2)
4) Wait till thermal equilibrium is achieved.
5) Standardise NaOH solution using oxalic acid solution 6) Pour 25 ml of 0.1 N HCl into each of the flasks (1
& 2)
7) Carefully add contents of flask one to two and immediately transfer from two to one .Place the conical flask
in temperature bath and at the same time start the stop watch
8) Pipette out 20 ml sample from the conical flask after 1.5 min and 2nd after 3 mints.
9) Back titrate against std 0.1 N HCl solution
10) Repeat the procedure for three different temperatures and intervals of at least 50 C.
Observation:
Normality of Ethyl acetate solution =0.1N
Normality of Hcl solution = 0.1N
Normality of NaOH solution = 0.1N
Normality of Hcl for titration = N3= 0.1N
Volume of sample =V2= ______ml
Volume of Ethyl acetate =V1= ______ml
Observation Table:
S.No Temp, oK Time (min) Vol of HCL CA 1/CA Kc lit/gm.mole.min LnKc 1/T, K-1
(ml)
1
2
3
4
5
Calculations:
CA = N1V1 – N3V3 / V2
Slope = E/R
1/CA
ln(k)
Time, (min)
1/T
Result: The value of activation energy = _____ Kcal

Experiment 6:
Investigate the molar flow rates of reagents entering the chemical reactors
by calibrating the peristaltic pump.
Objective: To calibrate the peristaltic pumps of the reagents to obtain the reagents molar flow rates.
Apparatus: Edibon QRC unit, 500 ml beakers, stop watch.
Chemicals: Ethyl Acetate (1liter 0.05M)
Sodium Hydroxide (1liter 0.05M)
Procedure:
Switch on the QRC unit and control software.
Place the outlet conduct of the reagent NaOH inside a millimeter glass of one liter capacity.
Activate the pumps and put the desired percentage in the software.
Calculate the time required to fill the 1 liter glass.
Repeat the same experiment for different percentages.
Repeat the whole previous procedure with the pump AB-2 & AB-3.
Results:
The given flow will be calculate as
𝑉
𝑄=
𝑡
As in our case the volume is 1 liter (tank volume), the flow will be calculated as:
1𝑙
𝑄=
𝑡[𝑚𝑖𝑛]
Represent the graph flow vs. percentages for the different reagents and save the results for the next practical
exercises.
Flow vs. Percentage

1.5
Q (Ltr/min)
0.5
0
0 0.5 1 1.5
Percentage, (%)
After calculating the volumetric flow rate, calculate the molar flow rates of caustic soda and ethyl acetate by
multiplying initial concentration with the volumetric flow rates.
FAo = Molar Flow rate of NaOH.
FBo = Molar Flow rate of Ethyl Acetate.
CAo = Initial Concentration of NaOH.
CBo = Initial Concentration of Ethyl Acetate.
Molar flow rate (NaOH) = FAo = VAo x CAo
Molar flow rate (EthOH) = FBo = VBo x CBo.
Experiment 7:
To carry out saponification of ethyl acetate in three CSTR’s in series and to
determine the conversion and to compare with single CSTR.
Objective: To study the conversion obtained in single and CSTR’s connected in series.
Apparatus: Edibon QRSC unit, 500 ml beakers, stop watch.
Chemicals: Ethyl Acetate (1liter 0.05M)
Sodium Hydroxide (1liter 0.05M)
Procedure:
Switch on the QRSC unit and control software.
Fill the reagents bottle with chemicals and marked them.
Check the CSTR’s connected in series, e.g. inlet and discharge pipes.
Activate the pumps and put the desired percentage in the software.
Observe the change in conductivities for three CSTR’s.
Results:
The given conversion be calculate as
𝐶𝐴𝑜 − 𝐶𝐴
𝑋=
𝐶𝐴𝑜
Similarly conversion in the following reactors can be calculated as above.
Represent the graph conversion vs. CSTR’s in series and save the results for the next practical exercises.
Conversion
CSTR's in series
Experiment-8
Determination of the ionic conductivities and temperature effect on
reagents conductivities.
Objective: The objective of this practical exercise is the determination of the ionic conductivities,
which are necessary for the treatment of the experimental data in next practical exercises.
Chemicals:
1liter solution of 0.05M Sodium Acetate.
1 liter solution of 0.05M Sodium Hydroxide.
QRC unit.
Procedure:
Introduce inside the reactor the solution of sodium acetate. Put the cap and adjust the stirrer. Run the
SACED-QUSC program. Select the option “Data Caprture”. Select the time of capture, select the name
of the file to the disk and finally press the play icon. Turn on the thermostatization of circuit and select
25oC. Turn on the stirring system to facilitate the quick thermostatization.
Take the sample in the lower mouth of the reactor and determine the conductivity of the solution at that
temperature. Repeat the measurements at 35 and 45oC. Take note of the results. Empty the reactor
through the inferior valve. Clean it with water several times. Repeat the precious steps with the solution
of sodium hydroxide. Clean the reactor again and switch off the system.
Temp (oC) κNaOH κEtONa Difference = (κ- κEtONa) NaOH x 10-3/ CAo
25
35
45
Conductivity
Temperature
Experiment-9
Obtain the reaction order for saponification reaction by integral method of
data analysis.
Objective:
𝑁𝑎𝑂𝐻 (𝐴) + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 (𝐵) → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

𝛽
−𝑟𝐴 = 𝑘𝐶𝐴∝ 𝐶𝐵
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 k0 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∞
=
𝐶𝐴𝑜 𝑘0 − 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]−
[𝑂𝐻]− = 10−𝑝𝑂𝐻
-
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.
THEORY
In theory part, write down something on integral method of data analysis.
PROCEDURE
Write down the procedure you followed when performing this experiment.
Results:
Time,(min) ‘κ,conductivity Concentration ‘ln(CA) ‘ln(CAo/CA) 1/CA
0
1
2
3
4
5
6
Graph:
6
, ln(CA), 1/CA, ln(Cao/Ca)
0
0 2 4 6 8 10
-1
Time, (min)
Experiment-10
Develop a stoichiometric table and plot conversion and concentration of
reactants and products for the kinetics on saponification of ethyl acetate.
Objective:

𝛽
THEORY
In theory part, write down something on stoichiometric table, why they are developed.
PROCEDURE
Write down the procedure you followed when performing this experiment.
𝐶(𝑡) 𝑘(𝑡) − 𝑘∞
=
Where,
Conversion can be calculated as
𝐶𝐴𝑜 − 𝐶𝐴
𝑋=
𝐶𝐴𝑜
The concentration of individual species can be calculated as

𝐶𝐴 = 𝐶𝐴𝑜 (1 − 𝑋)
𝑏
𝐶𝐵 = 𝐶𝐴𝑜 (Ɵ𝐵 − 𝑋)
𝑎
𝑐
𝐶𝐶 = 𝐶𝐴𝑜 (Ɵ𝐶 + 𝑋)
𝑎
𝑑
𝐶𝐷 = 𝐶𝐴𝑜 (Ɵ𝐷 + 𝑋)
𝑎
Results:
Symb Chan
Species Initial Remaining Concentration
ol ge
NaOH A NAO
CH3COOC2H5 B NBO
CH3COONa C NCO
C2H5OH D NDO
Graph:
0.12 1.2
0.1 1
Concentration, (CA, CB, CC, CD)
0.08 0.8
Conversion, (X)
0.06 0.6
0.04 0.4
0.02 0.2
0 0
0 2 4 6 8 10
Time, (min)
Experiment-11
Determine the specific reaction rate constant of saponification reaction.
Objective:

𝛽
𝐶(𝑡) 𝑘(𝑡) − 𝑘∞
=
Where,
Rate constant can be calculated as
Theory:- Integral method of data analysis.
𝑑𝐶𝐴
= 𝑘𝐶𝐴∝
𝑑𝑡
For First order kinetics integrate the equation at initial conditions. i.e. t = 0 , CA = CA0.
𝐶𝐴 𝑡
𝑑𝐶𝐴
∫ = 𝑘 ∫ 𝑑𝑡
𝐶𝐴
𝐶𝐴𝑜 0
𝐶𝐴𝑜
𝑙𝑛 ( ) = 𝑘𝑡
𝐶𝐴
The equation looks like y = mx+c
Plot ln(CAo/CA) vs. time to find the slope of the graph, which is the rate constant for the reaction.
time conduct concentration ‘ln(Cao/Ca)
ivity
0
1
2
3
4
5
6
7
8
Graph:
4
, log(Cao/Ca)
0
0 2 4 6 8 10
-1
Time, (min)

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Laboratory Manual

CHEMICAL REACTION ENGINEERING CHE-324

Department of Chemical Engineering

Week 10 Experiment-7 To carry out saponification of ethyl acetate in three CSTR’s in

Week 11 Experiment-8 (EDIBON Training Panel)

First Sessional Test 10%

Weeks 18-19 Terminal Examination

14. Format of Assignment

Instruction for Laboratory Teachers:

Figure 1 Laboratory Batch Reactor (EDIBON, Spain)

Figure 2 Continuous Stirred Tank Reactor (EDIBON, Spain)

Continuous Stirred Tank Reactor in Series:-

Plug Flow Reactor:-

Figure 4 Plug flow reactor (EDIBON, Spain).

2. Note that the total volume in each beaker is 25 mL.

Chemicals: 1 M hydrochloric acid

Run 1 Run 2 Run 3 Run 4

Volume of 1 M HCl(aq) (mL) 20 10 20 20

Volume of 1 M CH3COCH3(aq) (mL) 8 8 4 8

Volume of deionised water (mL) 0 10 4 2

Volume of 0.002M I2(aq) (mL) 4 4 4 2

[I2] in the time taken (mol dm-3)

Initial rate of reaction (mol dm-3 s-1)

5. Write the rate equation for the reaction.

Result: The value of activation energy = _____ Kcal

Flow vs. Percentage

𝑁𝑎𝑂𝐻 (𝐴) + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 (𝐵) → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

In theory part, write down something on integral method of data analysis.

Time,(min) ‘κ,conductivity Concentration ‘ln(CA) ‘ln(CAo/CA) 1/CA

𝑁𝑎𝑂𝐻 (𝐴) + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 (𝐵) → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

The concentration of individual species can be calculated as

𝑁𝑎𝑂𝐻 (𝐴) + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 (𝐵) → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

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