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CHEMICAL LABORATORY EXPERIMENTS

REACTION ENGINEERING

LABORATORY MANUAL

Lecturer/Instructor:

Name:
Student ID:
Course:

FACULTY OF ENGINEERING, ARCHITECTURE & BUILT


ENVIRONMENT

UCSI UNIVERSITY

TABLE OF CONTENT
General Instructions
Experiment 1

Batch Saponification Reaction of Et (Ac) and NaOH

Experiment 2

The Effect of Step Change Input

Experiment 3

The Effect of Pulse Input for CSTRs in series

Experiment 4

Pulse Input in a Plug Flow Reactor

Experiment 5

Develop Langmuir Adsorption Isotherm for The


Adsorption of Acid
APPENDIX
A Batch Reactor
B CSTRs in series
C Tubular Flow Reactor
D Calibration Curve for Batch Reactor

GENERAL INSTRUCTIONS
Laboratory experiments are designed with the intention of being
completed during the allotted classroom time. In order to expedite things it is
mandatory that you be prepared prior coming to the lab. This includes reading the
lab procedure handout thoroughly and understanding the experiments illustrations
and techniques.

In additional, any applicable calculations (such as solution

preparations) should be made in advance so that work may commence upon


arriving in the lab. A flowchart of the experiment methodology is helpful in
determining what steps should be taken and the order in which things must be
done. In addition, it is important that you familiarize yourself with lab techniques
learned in your chemistry classes.

Some experiments may take longer that the others, but the biggest
determinant will be your preparation.

ATTENDANCE IS MANDATORY!

(A)

Laboratory logbook

You are required to have a logbook. This must be a bound logbook. It is


very important to get into a habit of writing a logbook. You are required to
translate the procedure of each lab in the lab manual into graphical illustration or
flowchart in your logbook before you begin your experiment.
Recording in the logbook should be written as the experiment is carried
out and should be as brief, but concise, as possible. Record in your logbook
everything you do and observe as you carry out the experiment.
Each experiment in the logbook should contain the following information:

(i)

Title of the experiment

(ii)

Date of the experiment carried out

(iii)

Objective of the experiment

(iv)

Hypothesis of the experiment

(v)

Procedure outline or brief description of the method

(vi)

Observation (should be recorded throughout the experiment)

A logbook should be neat. Clarification of procedure and results are


important. Always use a pen to write your logbook. For any mistake or changing
of the data written on the logbook, the usage of liquid paper or eraser is not
allowed. Always use a pen to cross out if any errors.
The lab instructor/lecturer will inspect and sign your logbook during the
lab session and possibly grade them at the end of the semester.

(B)

Laboratory group

You will be assigned to a lab group (please refer to the student notice
board or outside the lab after the first session of the laboratory meet up). Students
are not allowed to change their team member for lab. You are required to work
with you group members as much as possible in terms of understanding the lab
work and sharing information on the different sections that were performed by
different members.

(C)

Laboratory reports
i)

Report submission

Report must be submitted one week after the scheduled experiment and
within the 1st 10 minutes of the due lab period. Marks would be deducted
accordingly for late reports or may not be accepted. Students who caught blatantly
copying from other or involved in any plagiarism activities will be required to
resubmit their work, or otherwise zero marks will be given.

ii)

Report style/format

Lab report must be in hand written or typed. Each of the group members
must contribute in the report. Report should contain the following:

Front page (refer the at Appendices A)


Table of content
Objective
Introduction/background of the experiment
Material and Methodology
Results and discussion
Conclusion
Limitation of the Experiment
Reference
Appendix (if any)

Lab reports are to be assembled in a logical and orderly way. Tedious


calculations must be placed in sequential order in the report. The report shall be:

(i)

Written in passive tense.


Example: Five milligram of solid was weighted.

(ii)

Graph must be with title, axis labels with units and legend when
necessary. The scale of the graph should be adjusted to fit the
graph data.

(iii)

Plagiarism will not be allowed and tolerated.

(iv)

Use suitable analysis method during explanations for the graph


such as R-value, slope of the line, line equations, etc in explaining
the experiment.

(v)

Only chemical compound structures can be drawn using


handwriting.

Report outlines and marks distributions:


Introduction/

3%

Background

Contain a concise summary of the experiment that is carried


out. Includes the statement of purpose, an introduction into
technique used and a brief overview of the instrumentation.

Material&

3%

Methodology

Contains all relevant experimental procedures, materials and


instrument parameters used in the analysis or during the
experiment.

Results&

5%

Discussion

-Show all the results from the experiment by using graph,


diagram, table, etc. All the data must be at appropriate
units. The calculation should shows in systematic basis.
Show only one example calculation for repeat data trials.
Include statistical analysis if any.

All results must be

expressed to correct significant figures and in correct units.


-Explanation of the figures or graph or data should followed
by supporting reference or relevant/logical analysis.
Conclusion

2%

Conclusion should reflect an understanding of the chemical

theory involved and achievement of the experiment


objective.
Limitation of

2%

It may include the limitation of the technique or

the

methodology of the experiment based on literature study.

experiment

Includes also any error that encounter during the experiment


is carried out. Suggest for improvement to avoid error.

Reference

3%

A minimum of 3 references should be cited in the


experiment report.

Format

2%

Front page, table of content, reference writing style, graph,


figure, table, etc.

(D)

Laboratory Rules

All the laboratory rules already learned will be applicable all the time and
the students are required to comply with all the rules when there are in the
lab.

1. Wear closed shoes, lab coat and eye protection (goggles) at all the time while
in the laboratory.
2. DO NOT wear bulky clothes or loose sleeves and long pants. Wear suitable
attire for lab work. Those with long hair do tie it before entering the lab.
(lecturer/instructor preserve the right to not allow student who not follow this
rule from enter the lab)
3. Switch off your hand phones.
4. Always be punctual.

Students who come later than 15 minutes will not

allowed to perform the experiment.

5. Eating and drinking in the lab are strictly prohibited in the lab.
6. Students must have a towel (for cleaning purposes), a logbook and their lab
manual during the lab session.
7. Clean your bench and return all the apparatus to their respective places before
you leave the lab.
8. Read the lab manual and understand the lab before you going to the lab.
9. Use only the amount of the reagents required. Avoid wastage.
10. Dispose of excess reagents as instructed, never return excess reagents into the
bottle.
11. Make sure you know where the following safety devices are: eyewash station,
emergency shower, fire extinguisher, fire alarm station.
12. Clean up the broken glass and report to the lab instructor or lecturer
immediately.
13. Always follow the instruction of the lab instructor or lecturer before start the
lab.
14. Do not casually dispose chemicals into the sink. Some chemicals may washed
down the sink, while others may require a different method of disposal. If a
chemical can go in the sink, be sure to wash it away rather than risk an
unexpected reaction between chemical 'leftovers' later.

EXPERIMENT 1: Batch Saponification of Et(Ac) and NaOH

OBJECTIVES
-

To carry out a saponification reaction between NaOH and Et(Ac) in a


batch reactor .

To determine the reaction rate constant.

PROCEDURES
1. Perform the general start-up procedures as in Appendix A.
2. To begin a batch reaction experiment, close valve V3 and V7, switch on
pump P2 and open valve V8 to obtain highest possible flow rate into the
reactor .Fill reactor R1 with 0.1 M Et(Ac) to 1-L volume .Stop pump P2 .
3. Switch on pump P1 and open V4 to obtain highest possible flow rate into
the reactor .Fill reactor R1 with the 0.1 M NaOH until solution reaches a
total of 2-L volume .Stop pump P1.
4. Switch on stirrer M1 and start the timer immediately.
5. Record the conductivity values at 1 minute interval.
6. Stop the experiment when the conductivity values remain constant (i.e.
steady state condition).
7. Open valve V10 and drain all the solution from the reactor into waste tank
B4.

ANALYSIS AND DISCUSSION


Solution mixture volume

= ____________

Initial concentration of NaOH in the reactor vessel

= ____________

Initial concentration of Et(Ac) in the reactor vessel

= ____________

Time, t
(min)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Conductivity
QI01 (mS/cm)

Concentration
NaOH, CA (M)

Conversion, X
(%)

ln CA

dCA/dt

ln dC A/dt

1. Use the sample table for data collection.


2. Plot a graph of conversion vs. time.
3. For an equimolar reaction with the same initial reactants concentration
( 0 = 0 ) , the rate law is shown to be :

- = ln (-

) = ln k + a ln

is the concentration of NaOH in the reactor at time t.


4. Plot a graph of ln (

) vs. ln and evaluate the slope and y-axis

intercept.
5. Determine the order of the reaction, and the rate constant, k from the slope
and the intercept values.

EXPERIMENT 2: The Effect of Step Change Input

OBJECTIVES
-

In this experiment a step-change input would be introduced and the


progression of the tracer will be monitored via the conductivity
measurements in all the three reactors.

PROCEDURES
1. Perform the general start-up procedures as in Appendix B.
2. Fill up the feed tank B1 with deionised water .Open V1 and V2.
3. Prepare about 30L of 0.025 M sodium chloride solution in feed tank B2.
4. Set the 3 way valve V5 position towards pump P1.Close valve V7.
5. Open valves V6 and V13 .Switch on Pump P1 to initially fill up all three
reactors with deionised water .Record each reactor volume.
6. Regulate the pump speed to obtain a flow rate of approximately 150
ml/min on flow meter FI01.Make sure that no air bubbles are trapped in
the piping and conductivity probe, hence will affect the reading.
NOTE: It is important to maintain the liquid level in each reactor .Adjust
the flow rate is necessary.
7. Switch on stirrers 1, 2 and 3 and set the speed 200 rpm.
8. Continue pumping the de-ionized water until all conductivity readings
(QI01,QI02 AND QI 03) are stable at low values. Make sure that the
overflow piping is free from the air bubble.
NOTE: Regulate the drain valve to make sure the solution flowing inside
the overflow tube.
9. Record these conductivity values at time, 0 .

10. Switch off pump P1 .Quickly set the 3 way valve V5 position towards
pump P2 .Switch on pump P2 and start the timer simultaneously.
11. Regulates the pump speed, to maintain the flow rate at 150 ml/min on flow
meter FI01.
12. Record all conductivity values (QI01,QI02 AND QI03) at a suitable
interval (e.g. 1 minute ) in an appropriate table.
13. Continue recording the conductivity values until all readings are almost
constant.
14. Switch off pump P2.Close valves V5.
15. Drain all liquids in each reactor by opening valves V10 to V14.

ANALYSIS AND DISCUSSION


Flowrate of Deionized water from tank

= _________

Flowrate of NaCl from tank

= _________

Speed of stirrer M1, M2 and M3

= _________

C0

= _________

Record the conductivity readings for the three CSTRs in series (QI01 ,QI02 AND
QI03 )
Time (min)
0
2
4
6
8
10
12

Q1 (mS/cm)

Q2 (mS/cm)

Q3 (mS/cm)

14
16
18
20
22
24
26
28
30
32
34
36

On the same graph, plot all 3 conductivity readings against time, together with the
step change input. Observe the transient behavior in the three CSTRs in series and
discuss.

EXPERIMENT 3: The Effect of Pulse Input for CSTRs in series

OBJECTIVES
-

In this experiment a pulse input would be introduced and the progression


of the tracer will be monitored via the conductivity measurements in all
the three reactors

PROCEDURES
1. Fill up the feed tank B1 with deionised water. Open V1 and V2.
2. Prepare about 30L of 0.025M Sodium Chloride solution in feed tank B2.
3. Set the 3-way valve V5 position towards pump P1. Close valve V7.
4. Open valve V6 and V13. Switch on pump P1 to initially fill up all three
reactors with deoinised water. Record each reactor volume.
5. Regulate the pump speed, P1 to obtain a flow rate of approximately 150
ml/min on flow meter FI01. Make sure that no air bubbles are trapped in
the piping, overflow tube and conductivity probe, hence will affect the
reading.
NOTE: It is important to maintain the liquid level in each reactor. adjust
the flow rate is necessary. If air trap inside the overflow tube, adjust drain
valve.
6. Switch on stirrers 1, 2 and 3 and set the speed to 200 rpm.
7. Continue pumping the de-ionized water until all the conductivity readings (QI01,
QI02 and QI03) are stable at low values.
8. Record these conductivity values at time, to
9. Switch off pump P1. Quickly set the 3-way valve V5 position towards pump P2.
Switch on pump P2 and start the timer simultaneously.
10. Regulates the pump speed, to maintain the flow rate at 150 ml/min on flow meter
FI01.

11. Let pump P2 run for 5 minutes and then switch off pump P2. Set the 3-way valve
V5 towards P1. Switch on pump P1 back and let it run till the end of experiment.\
12. Record all conductivity values (QI01, QI02 and QI03) at suitable interval (e.g 1
minute) in an appropriate table.
13. Continue recording the conductivity values until all readings are almost

constant.
14. Switch off pump P2. Close valves V5.
15. Drain all liquids in each reactor by opening valves V10 to V14.

ANALYSIS AND DISCUSSION


Flowrate of distilled water from tank

= ________

Flowrate of NaCl from tank

= ________

Speed of stirrer M1, M2 and M3


CO
Record the conductivity readings for the three CSTRs in series (QI01,
QI02 and QI03)

Time (min)
0
2
4
6
8
10
12
14
16
18

Q1 (mS/cm)

Q2 (mS/cm)

Q3 (mS/cm)

20
22
24
26
28
30
32
34
36

On the same graph, plot all 3 conductivity readings against time, together with the
pulse change input. Observe the transient behavior in the three CSTRs in series
and discuss. Thus, compare this experiment with previous experiment 2. What can
you discuss about both effect?

EXPERIMENT 4: Pulse Input in a Plug Flow Reactor

OBJECTIVES
-

To examine the effect of a pulse input in a plug flow reactor

To construct a residence time distribution (RTD) function for the plug


flow reactor.

PROCEDURES
1. Perform the general start up procedures as in Appendix C.
2. Open valve V9 and switch on pump P1.
3. Adjust P1 flow controller to give a constant flow rate of de-ionized water
into the reactor R1 at approximately 150 ml/min at F1-01.
4. Let the de-ionized water to continue flowing through the reactor until the
inlet (Q1-01) and outlet (Q1-02) conductivity values are stable at low
levels. Record both conductivity values.
5. Close V9 and switch off pump P1. Open valve V11 and switch on pump
P2. Start the timer simultaneously.
6. Adjust P2 flow controller to give a constant flowrate of salt solution into
the reactor R1 at 150 ml/min at FI-02.
7. Let the salt solution to flow for 1 min, then reset and restart the timer. This
will start the time at the average pulse input.
8. Then, close valve V11 and quickly open valve V9. Switch off pump P2.
9. Make sure the de-ionized water flow rate is always maintained at 150
ml/min by adjusting P1.
10. Start recording both the inlet (QI-01) and outlet (QI-02) conductivity
values at regular intervals of 30s.

11. Continue recording the conductivity values until all readings are almost
constant and approach the stable low level values.

ANALYSIS AND DISCUSSION

Flowrate

Input type

Time

Conductivity

(mS/cm)

Time

Conductivity

(mS/cm)

(min)

Inlet

Outlet

(min)

Inlet

Outlet

0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0

EP 319 CHEMICAL REACTION ENGINEERING AND DESIGN


MAY AUGUST 2015 SEMESTER
EXPERIMENT 5: DEVELOP LANGMUIR ADSORPTION ISOTHERM
FOR THE ADSORPTION OF ACID

You have been supplied with Acetic acid solution (1M) and an adsorbent (silica
gel/ activated carbon). Develop a laboratory procedure to find the Langmuir
adsorption isotherm for the adsorption of solute (acetic acid). Conduct the
experiments and develop the isotherm and analyze the parameters. NaOH (0.1M)
will be given for quantification of acid by titration method.
Present your results as a written report in which you provide the theory of
adsorption, Langmuir adsorption, full details of the procedure. In addition, the
report should also include the following points:
1.

Theory (adsorption, Langmuir isotherm)

2.

Materials and Methods for experiment

3.

Results (tables, graphs and parameters)

4.

Inference / conclusion from your experiment

APPENDIX A : BATCH REACTOR

General Start-up Procedures


1. Prepare the following solutions:
a) 15 liter of sodium hydroxide, NaOH (0.1 M) in tank B1.
b) 15 liter of ethyl acetate, Et (Ac) (0.1 M) in tank B2.
2. Ensure that all valves are initially closed except by-pass valves V3, V7
and V14.
3. Fill water bath tank B3 with water. Close the water bath tank.
4. Turn on the power for the control panel.
5. Switch on the stirrer M1 and adjust the knob to obtain a speed of 200 rpm.
Switch off the stirrer M1.
6. Open valves V2, V6 and V13.
7. The unit is now ready for experiment.
General Shut-down Procedures

1. Keep the cooling water to continue flowing.


2. Switch off pumps P1, P2 and P3. Switch off stirrer M1.
3. Switch off both heaters W1 and W2. Let the liquid in the reaction vessel
R1 to cool down to room temperature.
4. Turn off the power for the control panel.
5. Keep the solutions for subsequent experiment. Otherwise, open valves V1
to V8 to drain all solutions from feed tanks B1 and B2.
6. Open valves V10 to drain any liquid from reactor R1 into waste tank B4.

APPENDIX B : CSTR IN SERIES

General Start-up Procedures


1. Ensure all the valves are closed initially.
2. Prepare a 30-L of salt solution (e.g. sodium chloride, NaCl; 0.025 M).
3. Fill the feed tank B2 with the NaCl solution.
4. Turn on the power for the control panel.
5. Connect the water de-ionizer to the laboratory water supply. Open valve
V16 and fill up feed tank B1 with de-ionizer water. Close valve V16.
6. Open valve V3 and V6. Switch three way valve V5 to the left side towards
pump P2. Switch on pump P2. Regulate speed of pump to obtain a flow
rate of approximately 150 ml/min at flow meter FI-01. Switch off pump
P2. Drain all liquid from the three reactors.
7. Open valve V1. Switch three way valve V5 to the right side towards pump
P1. Switch on pump P1. Regulate speed of pump to obtain a flow rate of
approximately 150 ml/min at flow meter FI-01. Allow the de-ionized
water to overflow from reactor R3 until the conductivity value stabilizes at
low value. Switch off pump P1.
Note: Make sure there is no bubble trap inside the overflow reactor, if air
bubble blocks the flow, regulate the drain valve.
8. The unit now is ready for experiments.

General Shut-down Procedures

1. Switch off both pumps P1, P2. Close valves V1 and V3.
2. Open valves V10 to V14 to drain all liquid into waste tank.
3. If the equipment is not going to be used for long period of time, drain all

liquid for both feed tanks by opening valves V1 to V5. Rinse the feed
tanks with clean water.
4. Turn off the power for the control panel.

APPENDIX C : TUBULAR FLOW REACTOR


General Start-up Procedures

1. Ensure that all valves are initially closed except valve V7.
2. Prepare a 20 liter of salt solution (e.g. sodium chloride, NaCl; 0.05 M).
3. Fill the tank B2 with the NaCl solution.
4. Connect the water de-ionizer to the laboratory water supply. Open valve
V19 and fill up feed tank B1 with the de-ionized water. Close valve V19.
5. Turn on the power for the control panel.
6. Open valves V2 and V10. Switch on pump P1. Adjust P1 to obtain a flow
rate of approximately 150 ml/min at flow meter FI-01. Close valves V10
and switch off pump P1.
7. Open valves V6 and V12. Switch on pump P2. Adjust P2 to obtain a flow
rate of approximately 150 ml/min at flow meter FI-02. Close valves V12
and switch off pump P2.
8. The unit is now ready for experiment.

General Shut-down Procedures


1. Switch off both pumps P1, P2 and P3. Close valves V2 and V6.
2. Switch off the heaters.
3. Keep the cooling water circulating through the reactor while the stirrer

motor is running to allow the water jacket to cool down to room


temperature.
4. If the equipment is not going to be used for long period of time, drain all

liquid from the unit by opening valves V1 to V16. Rinse the feed tanks
with clean water.
5. Turn off the power for the control panel

Calibration Curve For Batch Reactor

Conversion
0%
25%
50%
75%
100%

Solution Mixtures
0.1 M NaOH
0.1 M Na(Ac)
100 mL
75 mL
25 mL
50 mL
50 mL
25 mL
75 mL
100 mL

Concentration
of NaOH (M)

Conductivity
(mS/cm)

0.05
0.0375
0.025
0.0125
0

12
8.6
6
4
0.5

H2O
100 mL
100 mL
100 mL
100 mL
100 mL

Conductivity vs Conversion
14
Conductivity (mS/cm)

12
10
8

y = -11.04x + 11.74
R = 0.992

6
4
2
0
0%

20%

40%

60%
Conversion (%)

80%

100%

120%