LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)

LABORATORY REPORT GUIDELINES

Each experimental report should contain the following items in accordance to the numbering as
listed:
1. COVER PAGE
Please insert the LABORATORY REPORT SUBMISSION FORM as the front cover.
DOWNLOAD FROM VLE.

2. TABLE OF CONTENTS
The table of content and number of pages should be in following format.
Note: Each page should be numbered.
Content Page Number
Summary
1.0 Results and Discussion
2.0 Conclusions and Recommendations
3.0 Tutorial
4.0 References
5.0 Appendices

3. SUMMARY
Give the summary (not more than half page) on the overall experimental report. Give brief
review on the objectives of the experiment, main experimental results and discussions which
are deemed significant and finally conclusions obtained from the work.

4. RESULTS AND DISCUSSIONS

Note: Refer to the respective experimental procedure (Analysis and Discussion
sections) to determine the extent of analysis and discussions required.
a. Record down and present each of the experimental data and findings in proper manner.
b. Present the data either in Table, Graph, Histogram or Pie chart form as deemed suitable
with complete label and units.
c. Explanations of the referred table and figure must be presented below the table and figure.

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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
Example Table:
Table 1: X vs. Y
Samples X (unit) Y (unit)
A
B
C
D

Example Graph:
2.0

1.8

1.6

1.4
Parameter Y (unit)

1.2

1.0

0.8 y = -0.7886x + 1.7986

0.6

0.4

0.2

0.0
0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6
Parameter X (unit)

Figure 1: Relationship between X and Y

d. Based on the experimental results, discuss on your findings and relate to your theory and
objective of experiment

7. CONCLUSIONS AND RECOMMENDATIONS

a. Summary of the results to relate briefly the findings or results with the theory applicable
to the experimental
b. Suggest improvements in apparatus or measurement procedure, or even experimental
procedures for future work (if applicable).
c. Should be in one paragraph.

8. TUTORIAL
Tutorial are the questions as given in the laboratory procedures. All questions must be
answered as required or else marks would not be rewarded for this section.

9. REFERENCES
Details of published sources of material referred to or quoted in the text (including any lecture
notes and URL addresses of any websites used).

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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
REFERENCES SHOULD BE IN COMPLETE FORM AS GIVEN BELOW OR ELSE MARKS WILL
BE DEDUCTED FOR EACH ERROR.
A. The references should be in following format:
1. Books/Journals: Authors (editor), title, publisher, year, chapter or page number
Example:
Smith J.M. and Van Hess H.C., Introduction to Chemical Engineering
Thermodynamics, McGraw-Hill, New York, 2001, p229
2. Internet Website: Title of the information, year, source of data, [Online]. [Date
Accessed]. Available from World Wide Web
Example:
BP Statistical Review of World Energy, 2007, BP (British Petroleum), [Online].
[Accessed 19th January, 2008]. Available from World Wide Web:
http://bp.com/statisticalreview.
B. The references should be arranged according to the author name in alphabetical order.

10. APPENDICES
All the raw data and sample of calculations should be included here.
Note: students are given option to handwrite the calculations part as tasked in the report.
However, the other part of the report should be typed.

IMPORTANT NOTE:
1. Laboratory reports are meant to be group tasks.
2. Any information copied from another group or taken directly from other sources such as Internet
without proper references will not be tolerated and the report will be marked as zero.
3. Laboratory report should be submitted directly to the lecturer in charge for date verification.

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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)

APPENDIX
CHEMICAL PREPARATION

1. Ethyl acetate (CH3COOCH2CH3) (Liquid Phase)

Volume of ethyl acetate needed, V1 (L) from the original solution
æ mol ö
M2 ç ÷V2 (L)
è L ø
V1 (L) =
æ mol ö
10.10 ç ÷
è L ø
Where;
M2 = Desired molarity of Ethyl Acetate (mol/L) required in the experiment
V2 = Desired volume of Ethyl Acetate (mol/L) required in the experiment

2. Sodium Hydroxide (NaOH) (Solid Phase)

Weight of NaOH required for experiment, mNaoH

æ mol ö æ g ö
mNaOH (g) = M 2 ç ÷ ´ MWNaOH ç ÷ ´V2 (L)
è L ø è mol ø
Where;
M2 = Desired molarity of NaOH (mol/L) required in the experiment
V2 = Desired volume of NaOH (mol/L) required in the experiment
Molecular weight of NaOH, MW NaOH = 40.0 g/mol

3. Hydrochloric acid (HCl) (Liquid Phase)

Volume of hydrochloric acid needed, V1 (L) from the original solution
æ mol ö
M2 ç ÷V2 (L)
è L ø
V1 (L) =
æ mol ö
1.0 ç ÷
è L ø
Where;
M2 = Desired molarity of HCl (mol/L) required in the experiment
V2 = Desired volume of HCl (mol/L) required in the experiment
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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)

LABORATORY MANUAL
CHEMICAL PROCESS PRINCIPLES
CLB 12004

JULY 2017

LIST OF EXPERIMENTS:

EXPERIMENT 1: BATCH REACTOR

EXPERIMENT 2: CONTINUOUS STIRRED TANK REACTOR (CSTR)

EXPERIMENT 3: DRYING PROCESS

EXPERIMENT 4: SHELL AND TUBE HEAT EXCHANGER

EXPERIMENT 5: DISTILLATION PROCESS

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EXPERIMENT 1
BATCH REACTOR

OBJECTIVES

To conduct mass balance and energy balance in batch process system

1.0 GENERAL DESCRIPTION

1.1 Description and Assembly

Before operating the unit and running experiments, you must familiarize yourself with
the unit’s components. Please refer to Figure 1 to understand the process. All glass
components of the QVF Batch Reactor unit are made of borosilicate glass with PTFE
gaskets.

1. Reactor (R1)

 Fused jacketed vessel with graduation, nominal capacity 10 L

 Bottom port for dead space reduced bottom outlet valve

 Jacket connections for heating agent

 Cover DN300 with connections for: Agitator

 Charge port with screw cap for feeding by hand

 Inlet for dosing vessel B1

 Vapour pipe with connection for distillate and vapour trap

 Conductivity and temperature sensor

2. Agitator (A1)

 Laboratory drive 230V / 50,60Hz

 0.25 kW, 0-550 rpm, steplessly adjustable by hand

3. Dosing vessel (B1)

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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
 2,000 mL graduated cylindrical vessel with overflow pipe

4. Condenser (W1)

 Coil heat exchanger, area 0.3 m2

 Max coolant pressure of 3 bars with allowable temperature difference of 130°C

5. Instrumentation

 Temperature measurement (TI-101)

 Conductivity measurement (QI-401)

Figure 1: Batch Reactor Unit

Chemical engineering processes can be broadly divided into two types: batch processes and
continuous processes. In a batch process, input materials are placed in a reactor and product is
withdrawn some time later. This is typical of what is normally done in chemistry laboratories. You
will be studying for batch conditions the reaction between an ester (ethyl acetate) and sodium
hydroxide:

CH3 COOC2 H 5  OH  CH3COO  C 2 H 5 OH

This type of reaction is called a saponification because of its importance in the manufacture of soap.

The reaction is relatively slow and the changing ester concentration can be followed quite easily by
analyzing samples from the reaction mixture every few minutes.

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1.2 Safety Considerations

1. Students must not carry out laboratory work without the supervision of a lecturer.
2. Read operating instructions carefully, and make sure that you fully understand all
aspects of operation of the batch reactor unit.
3. Safety glasses must be worn at all times during these experiments – remember
you are in charge of all safety aspects.
4. For each experimental setting, allow 10 minutes for equilibrium conditions to be
established.
5. After each experiment, make sure that the reactor and tubing are cleaned properly.
Sodium hydroxide and ethyl acetate both are corrosive and can damage the
tubing’s and the reaction rig.
6. Dispose all liquids immediately after each experiment. Do not leave any reactants
or product in the feed or product vessels.
7. Wipe off any spillage on the ground or working bench.
8. Plastic gloves and eye shields must be worn when handling corrosive liquids, and
heat resistant gloves when adjusting steam valves.
9. All experiments involving a potential explosive hazard must be conducted behind
special shields.
10. When working with solvents etc., ensure that the apparatus is adequately vented.
11. All used solvent should be handed to the technician and not disposed into drains
or laboratory sinks.
12. Smoking is forbidden in all laboratories.
13. Safety helmets must be worn.
14. Services equipment (vacuum generators) must in no circumstances be started up
by students.
15. Gas cylinders, when in use, should be adequately strapped to bench and
supported in the upright position, away from sunlight or flames. Ensure that
cylinders are shut-off after use.
16. Before using any chemical, ensure that you are familiar with its hazards and with
emergency procedures.
17. If in doubt, ask the lecturer in charge.
18. If chemical spillage occurs, evacuate the laboratory in an orderly fashion.
19. Plug in all cables into appropriate sockets before switching on the main switch.
Inspect all cables for any damage to avoid electric shock. Replace if necessary.

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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
20. Do not switch on the heater unless it is fully submerged in the liquid. Always
maintain liquid level above the height of the heater to avoid damage to the heater.

Batch Saponification Reaction

2.0 EXPERIMENTAL PROCEDURES

1. Prepare the following solutions:

a) 3 L of sodium hydroxide, NaOH (0.1 M)
b) 3 L of ethyl acetate, Et (Ac) (0.1 M)
2. Ensure that all valves are initially closed.
3. Turn on the power for the control panel.
4. Check that there is sufficient water in the thermostat T1 tank. Refill as necessary.
5. Open cooling water valve V5 and let the cooling water flow through the condenser W1.
6. Switch on the thermostat T1 and set the water temperature to the desired temperature.
7. The unit is now ready for experiment.
8. Measure and carefully pour 3 L of 0.1 M ethyl acetate solution into the reactor R1 through
the charge port on the vessel cover.
9. Then, measure and carefully pour 3 L of 0.1 M sodium hydroxide solution into the reactor
R1 through the charge port on the vessel cover.
10. Switch on the stirrer M1.
11. Start the timer simultaneously.
12. At every 5-minute interval, open sampling valve V1 (at the bottom) and collect a 10 mL
sample. Carry out a conductivity measuring by using conductivity meter.
13. Record your conductivity value and temperature value from TI-101 in the Appendix C.
14. End the experiment when the conductivity values do not change significantly over time.
Switch off the stirrer M1. Drain the reactor R1 by opening valve V1.
15. Perform the general shutdown procedures.

6.0 General Shutdown Procedures

1. Keep the cooling water valve V5 open to allow the cooling water to continue flowing.
2. Switch off the thermostat T1. Let the liquid in the reaction vessel R1 cool down to room
temperature.
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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
3. Switch off the stirrer M1.
4. Close cooling water valve V5. Open bottom valve V1 to drain any liquid from the unit.
5. Turn off the power for the control panel.

7.0 Analysis and Discussions

1. Use the sample table in Appendix C for data collection.

2. Find the concentration of NaOH in the reactor from the calibration curve. Subsequently
calculate the conversion, X based on the formula given in Appendix.

3. Plot a graph of conversion, X vs. reaction time, t. Discuss the plot.

4. Perform mass balance and energy balance for the batch reactor based on the
experimental results.

5. Subsequently, perform mass balance and energy balance for the batch reactor using
software (e.g. Microsoft Excel, etc.).

8.0 TUTORIAL
1. Describe an example of industrial applications other than saponification that utilized batch
reactors in its process. Discuss the advantages and disadvantages of using batch
reactors in chemical reaction.
2. Write a one-paragraph summary of any journal article that studies chemical reaction in a
batch reactor. The article must have been published within the last 5 years. Explain on
the batch reactor used in the study and its significance to the study done.

9.0 REFERENCES
1. Atkins, P.W. ‘Physical Chemistry’ (various ed.)
2. Smith, J.M. ‘Chemical Engineering Kinetics ‘(3rd ed.), McGraw-Hill, 1981
3. Frost, A.A. & Pearson, R.G. ‘Kinetics and Mechanics’ (2nd ed.), Wiley, 1961
4. Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd edition, Prentice Hall Int.
Series, N.J. (USA), 1997.
5. Levenspiel, O., Chemical Reaction Engineering, 3rd edition, John Wiley and Sons, 1999
6. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.
7. Model SOLTEC BP 141 Operating Manual, Solution Engineering Bhd, KL.

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APPENDIX B

TABLE OF CALIBRATION CURVE

Concentration Conductivity
of NaOH (M) (mS/cm)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental product (M) from
the pre-determined conductivity found during the experiment.

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APPENDIX C
Volume of NaOH = 3L
Volume of Et(Ac) = 3L
Temperature = _____ C
Concentration of Conversion,
Time Temperature Conductivity NaOH, CNaOH (M) X (%)
(min) (°C) (mS/cm) (From calibration (Self
curve) calculation)
0
5
10
15
20
25
30
35
40
45
50
55
60

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the measured
conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

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EXPERIMENT 2
CONTINUOUS STIRRED TANK REACTOR (CSTR)
OBJECTIVES
To conduct mass balance and energy balance in CSTR

1.0 GENERAL DESCRIPTION

1.1 Description & Assembly
Before operating the unit and running experiments, you must familiarize yourself with
the unit’s components. Please refer to Figure 2 to understand the process. All glass
components of the QVF Continuous Stirred Tank Reactor unit are made of borosilicate
3.3 glass with PTFE gaskets.

1. Reactor (R1)
 Fused jacketed vessel with graduation, nominal capacity 10 L
 Bottom port for dead space reduced bottom outlet valve
 Jacket connections for heating agent
 Cover DN300 with connections for:
Agitator
Charge port with screw cap for feeding by hand
Inlet for feed vessels B1 and B2
Vapour pipe
Integrated conductivity and temperature sensor
2. Agitator (A1)
 Laboratory drive 230V / 50,60Hz
 0.11 kW, 50-700 rpm, steplessly adjustable by hand, max torque 60 Ncm
3. Feed vessels (B1/B2)
 50 L graduated cylindrical vessels
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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
4. Pumps (P1/P2)
 Centrifugal pumps
 Max suction height of 3 m
5. Condenser (W1)
 Coil heat exchanger, area 0.2 m2
 Max coolant pressure of 2 bar with allowable temperature difference of 150°C
6. Receiving vessel (B3)
 100 L rectangular tank
7. Instrumentation
 Flow measurement (FI-301, FI-302)
 Temperature measurement (TI-101)
 Conductivity measurement (QI-401)

1.2 Safety Considerations

1. The unit must be operated under the supervision of an authorized staff who has
been properly trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
3. Feed stock which severely affects PTFE, PFA and borosilicate glass are not to be
used.
4. The system should not be subjected to shock, sudden impact, vibration, additional
load, or permanent external action of aggressive vapours.
5. Always check and rectify any leakages.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
10. Do not exceed the maximum cooling pressure of 2 bar (g) for the top condenser
(W3) and product cooler (W4).
11. Only a properly trained staff should be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
12. Before any servicing, shut down the whole operation, let the system cool down and
be properly ventilated.
13. Do not use any coarse or abrasive cleaners on glass components.
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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)
14. Leaking couplings should be carefully retightened. Replace any gaskets or seals if
necessary.

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LABORATORY MANUAL (JUL 2017) CHEMICAL PROCESS PRINCIPLES (CLB 12004)

Vent

V1 V6

Cooling
Water
B1 B2 W1 Cooling
Water
V13
HS
1

Q1
M 401

TI
101
V2 V7
FI FI
301 302

V5 V10 R1
V3 V8
V3

V11
V4 V9
P1 P2
M M V12
HS HS
2 3 B3 T1

Figure 2: Continuous Stirred Tank Reactor Unit

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Laboratory manual CLB 12004-Chemial Process Principles

2.0 OPERATING PROCEDURES

2.1 General Start-up Procedures

1. Prepare the following solutions:

a) 30 L of sodium hydroxide, NaOH (0.1 M)

b) 30 L of ethyl acetate, Et(Ac) (0.1 M)

2. Ensure that all valves are initially closed.

3. Charge the feed vessels as follows:

a) Open the charge port caps for vessels B1 and B2.

b) Carefully pour the NaOH solution into vessel B1 and the

Et(Ac) solution into vessel B2.

c) Close the charge port caps for both vessels.

4. Turn on the power for the control panel.

5. Open valves V2, V7, and V11.

6. The unit is now ready to be used for an experiment.

2.2 General Shutdown Procedures

1. Keep the cooling water valve V13 open to allow the cooling water
to continue flowing.

2. Switch off both pumps P1 and P2. Switch off the stirrer M1.

3. Switch off the thermostat T1. Let the liquid in the reaction vessel
R1 cool down to room temperature.

4. Close cooling water valve V13.

5. Open valves V4, V9 and V12 to drain any liquid from the unit.

6. Turn off the power for the control panel.

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Reaction in a CSTR
3.0 Experimental Procedures

1. Perform the general start-up procedures.

2. Check that there is sufficient water in the thermostat T1 tank.
Refill as necessary.
3. Open cooling water valve V13 and let the cooling water flow
through the condenser W1.
4. Switch on the thermostat T1 and set the water temperature to
the desired temperature.
5. Switch ON both pumps P1 and P2 simultaneously.
6. Open and adjust the valves V5 (Monitor at FI-301) and V10
(Monitor at FI302) to give the desired flow rate (flowrate: 200-
450 mL/min). Both must be adjusted to equal flow rate. Let the
reactor fill up with both solutions until it is just about to 1/2 full.
7. Switch ON the stirrer M1.
8. Adjust the valves V5 and V10 to give the desired flow rate.
Make sure that both flow rates are maintained the same.
9. Start monitoring the conductivity value at QI-401.
10. Start the timer and record the conductivity value (QI-401) and
both flow rates (FI-301 and FI-302) when it has reached
steady state (Conductivity value begin to steadily decline with
time).
11. Record the conductivity values and both flows rate for every 5
minutes until the conductivity does not change over time. This
is to ensure that the reactor has reached steady state.
12. End the experiment when the conductivity values do not
change significantly over time.
13. Perform the general shut-down procedures.

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4.0 Analysis and Discussions

1. Use the table for data collection at Appendix B.

2. Find the concentration of NaOH in the reactor from the calibration

curve. Subsequently calculate the conversion, X based on the formula
given in Appendix.

3. Plot a graph of conversion, X vs. reaction time, t. Discuss the plot.

4. Perform mass balance and energy balance for the CSTR based on the
experimental results.

5. Subsequently, perform mass balance and energy balance for the

CSTR using software (e.g. Microsoft Excel, etc.).

5.0 Tutorial

1. Discuss the advantages and disadvantages of using CSTR reactors in

chemical reaction. Describe an example of industrial applications that
utilized CSTR reactors in its process.

2. Write a one-paragraph summary of any journal article that studies

chemical reaction in a CSTR. The article must have been published
within the last 5 years. Explain on the CSTR reactor used in the study
and its significance to the study done.

6.0 References
1. Levenspiel O., “Chemical Reaction Engineering”, John Wiley (USA),
1972.
2. Fogler H.S., “Elements of Chemical Reaction Engineering, 3rd Ed.”,
Prentice Hall (USA), 1999.
3. Smith J.M., “Chemical Engineering Kinetics”, McGraw Hill (Singapore),
1981.
4. Astarita G., “Mass Transfer with Chemical Reaction”, Elsevier, 1967.

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APPENDIX A
RESULTS FOR PREPARATION OF CALIBRATION CURVE

Concentration Conductivity
of NaOH (M) (mS/cm)

0.0500 10.7
0.0375 9.7
0.0250 7.5
0.0125 5.6
0.0000 4.0

NOTE
1. Plot the calibration curve of concentration of NaOH (M) (x-axis) vs
conductivity (y-axis).
2. Determine the slope of the curve.
3. Use the calibration curve to determine the concentration of the experimental
product (M) from the pre-determined conductivity found during the
experiment.

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APPENDIX B
RESULTS FOR EXPERIMENTS

Total flow rate Concentrati

Flow rate of of solutions, on of NaOH, Conversion,
Temper Flow rate of
NaOH, F0 (mL/min), Conductivity CNaOH (M) X (%)
Time ature Et(Ac), FEt
FNAOH = FNAOH + FEt (mS/cm) (From (Self–
(°C) (mL/min)
(mL/min) (Self– calibration calculation)
calculation) curve)
0
5
10
15
20
25
30
35
40
45
50
55
60

Reactor volume= 10 L
Flowrate = _____ mL/min
Temperature = _____ oC

NOTE:
1. Obtain the concentration of NaOH for each of the reaction time from the
measured conductivity value based on the calibration curve (Appendix B).
2. Formula to calculate conversion, X
𝐶𝑁𝑎𝑂𝐻(𝑡=0)− 𝐶𝑁𝑎𝑂𝐻(𝑡)
𝑋= × 100%
𝐶𝑁𝑎𝑂𝐻(𝑡=0)

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EXPERIMENT 3
DRYING PROCESS
OBJECTIVES
To conduct mass balance and energy balance in drying process
To compare the experimental results and the predicted results from
software

1.0 INTRODUCTION

A large number of manufacturing processes necessitate the Drying of a

product or material and the equipment used in these industrial operations depends
on the particular process and type of material being dried. For example, the
requirements for Food Processing are more stringent than for Agricultural Fertilizer
materials, and the design of Driers for these purposes will be dictated by the
relative importance of such factors as Heat Sensitivity, Porosity, Bulk Density and
Particle Size of the dried material. In fact, since the Dried Solid is generally a
valuable product, it shape, colour, stability, stickiness and hence its overall sale
ability, all depends upon the Drying processes to which it has been subjected.

Although there are many different types and operating characteristics of

Industrial Driers, the SOLTEQ Tray Drier (Model: BP 772) has been designed to
provide an experimental facility based on one of the most fundamental designs.
Drying involves the transfer of liquid from a Wet Solid to an unsaturated gas phase
such as air, and the solid itself can exert a considerable influence on the Drying
process. The equipment enables the Basic Principles of Drying to be investigated
and students of Process Engineering may examine the problems of Fluid
Mechanics, Surface Chemistry, Solid Structure and Mass Heat Transfer
associated with general Drying behavior.

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Immediately after contact between the Wet Solid and the Drying Medium, the solid
temperature will adjust until it reaches a Steady State. The solid temperature and
the Rate of Drying may increase or decrease to reach the Steady State condition.
At Steady State, the temperature of the Wet Solid surface is Wet Bulb Temperature
of the Drying Medium. Temperature within the Drying Solid also tends to equal
the Wet Bulb Temperature of the gas but lag in movement of mass and heat result
in some deviation. Once the Stock Temperatures reach the Wet Bulb Temperature
of the gas, they are quite stable and the Drying Rate also remains constant. This
is the constant Rate Drying period, which ends when the solid reaches the Critical
Moisture Content. Beyond this point, the Surface Temperature rises, and the
Drying Rate falls off rapidly. The falling rate period can take a far longer time than
the constant rate period even though the moisture removal may be less. The
Drying Rate approaches zero at some equilibrium Moisture Content which is the
lowest Moisture Content obtainable with the Solid under the Drying condition used
the Moisture Content ( X ) of a Wet Solid is measured in terms of the weight of
moisture per unit weight of Dry Material. When a Wet Material of initial Moisture
Content, Xi is dried in a Tray Dryer, the typical variation of Moisture Content with
time is as shown in the diagram below.

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Laboratory manual CLB 12004-Chemial Process Principles

The equipment of SOLTEQ Tray Drier (Model: BP 772) comprise of an air

duct mounted on a floor standing frame to give a comfortable working height for
the operator. Air is drawn into the duct through a Mesh Guard by a motor driven
axial flow Fan Impeller whose speed can be controlled to produce a range of air
velocities up to 2.0 m/s in the duct. The air passes over an electrically heated
element controlled by a power regulator to provide a variation in air temperature
up to a maximum of 80°C at low air velocities.

The air passes into the central section of the duct where trays of material to
be dried are suspended in the air stream. The trays are carried on a support frame,
which is attached to a digital balance, mounted above the duct and on which the
total weight is continuously indicated. The trays are inserted or removed from the
duct through a latched side door with a glass panel for viewing purpose.

After passing over Drying Trays, the air is discharged at atmosphere

through an outlet duct section where a Vane Anemometer can be position. Wet
and Dry Bulb temperatures of the air are measured using a DC powered aspirated
Psychrometer. Access points for the Psychrometer are provided both upstream
and downstream of the Drying Trays and are covered by flaps when not in use. A
Process Flow Diagram for Tray Drying Process Unit is as shown below (Figure
3).

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Figure 3 : Tray dryer

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1.0 MATERIALS AND ANCILLARY EQUIPMENTS REQUIRED

a) Materials Required.
 Dry Sand.
 Water

b) Ancillary Equipments Required:

 One 2000ml beaker
 Empty Tray.

2.0 EXPERIMENTAL PROCEDURES

2.1 General Start-up:
2.1.1 Check that mains switch and other switches are in the OFF positions.
Connect the equipment to the electrical supply.
2.1.2 Remove the fan casing from the main body of the aspirated
Psychrometer (in the following diagram). Fill the wick chamber with
distilled water and make sure that the wick is immersed. Reassemble
the fan casing to the main body.
2.1.3 Insert the Psychrometer into the Upstream slot and connect the plug to
the DC socket at the control panel. Check that the electrical fan within
the Psychrometer operates and observe that the Dry and Wet Bulb
Temperatures are indicated satisfactorily on the Thermometers.
2.1.4 Remove the plug from the DC socket and check that the electrical fan
switches off.

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Note:
In Normal Operation, the Inlet Duct of the Psychrometer is inserted into the tunnel
through aperture Upstream or Downstream of the working section. These
apertures are shielded to prevent loss of air when the Psychrometer is not in use.

 Close the tunnel access door. Press the fan ON/OFF switch, rotate the fan
speed control knob clockwise and check that the fan speed adjusts
accordingly.
 Switch on the Digital Anemometer and read the Air Speed in different units.
Switch off the Digital Anemometer.
 With the fan operating, press the Heater ON/OFF switches, rotate the power
control knob clockwise and check that the air is heated by the electrical
elements Downstream of the fan.
 Set the fan and heater switches to the OFF position. Press the ON/OFF
button on the Digital Balance and observe the digital reading. Check
operation of the tare (without any weight, blank) control of the balance and
adjust to give a simple number on the display. Open the access door and
place a suitable weight on the Sample Trays. Check correct operation of the
balance. Remove the weight from the Sample Tray and check balance
returns to original reading.

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Note:
It is recommended that the laboratory be well ventilated to ensure that warm moist
air discharge from the Drier does not affect the original inlet conditions during the
period of the experiments.

2.2 Procedures:
2.2.1 Fill the tray to a depth of about 10 mm of dry sand and measure the
weight of the sand accurately.
2.2.2 Spray water until the sand is saturated with water.
2.2.3 Remove the sand from the tray and drain of excess free water before
being loaded evenly a smoothly into the drying trays, taking care to avoid
spillage.
2.2.4 Record accurately the total weight of wet sand.
2.2.5 At some arbitrary time (t = 0), switch on the fan and set the speed control
to mid position.
2.2.6 Switch on the heater and set the power control to maximum, letting them
remain constant throughout the experiment.
2.2.7 Record the total weight of sand in the tray at regular time intervals which
is for every 5 minutes in the provided table of results until the reading is
constant or the drying is complete.

2.3 General Shut – Down:

2.3.1 Remove the tray with the dried sand from the tray.
2.3.2 Switch off the fan and heater.
2.3.3 Switch off the power supply.

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3.0 Result and Discussion

Discuss all your results. The questions below only serve as a guideline. Your
discussion should not only limit to these questions.
1. Perform the mass balance and energy balance for the equipment.
2. Perform the mass balance and energy for the equipment using software
(e.g. Microsoft Excel, etc.)

Table of Results:
Weight of Empty Tray = ______________ g
Weight of Dry Sand and Tray = ______________ g
Weight of Dry Sand = ______________ g
Weight of Wet Sand and Tray = ______________ g
Weight of Wet Sand = ______________ g
Air Velocity = ______________ m/s

Table 1:

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Time Mass of Total Inlet (oC) Outlet (oC)

(min) wet sand moisture Dry Wet Dry Wet bulb
(g) content, bulb bulb bulb
XT
0

Table 2:

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Time, t Free Moisture

Content, X

4.0 Useful Information

1. Total moisture content, XT

m  ms
XT 
ms

m : mass of wet sand

ms : mass of dry sand

2. Free moisture content, X

X  XT  X *
X* : equilibrium moisture content
A : area of tray (540 cm2)
5.0 Tutorial

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1. Discuss the advantages and disadvantages of using tray dryer in drying

process. Describe an example of industrial applications that utilized tray
dryer in its process.
2. Write a one-paragraph summary of any journal article that studies drying
process. The article must have been published within the last 5 years.
Explain on the drying equipment used in the study and its significance to
the study done

6.0 References
1. Geankoplis, Transport process and unit operation 3rd Edition, Prentice
Hall (1993).
2. McCabe, Smith and Harriott, Unit operations of Chemical Engineering,
McGraw Hill 6th edition (2000).

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EXPERIMENT 4

SHELL AND TUBE HEAT EXCHANGER

OBJECTIVES
• To evaluate and study the performance of the shell and tube heat exchanger at various
operating conditions.

• To perform mass and energy balance in Shell and Tube Heat Exchanger.

OVERVIEW

The most common heat exchanger is shell and tubes heat exchanger, where bundles of tubes
arranged inside the shell or even mo-e shell. This heat exchanger possesses a heat transfer
area of 31.67 ft2. The proper arrangement of tube inside the heat exchanger shell allows
ultimate heat transfer between the fluid in tube side and shell side. This phenomenon can
be studied by flowing two types of different temperature fluid through the shell and tube
respectively. This experiment will determine the total heat transferred between the shell and
tube side and evaluate the overall heat transfer coefficient U for this heat exchanger.
Meanwhile, the pressure drop for the fluid flow in the shell and tube side will also be observed
and recorded.

1. INTRODUCTION

To design a shell and tube heat exchanger, it is necessary to relate the total heat transfer rate
to fluid temperature (inlet and outlet), overall heat transfer coefficient (U) and the total surface
area for the heat transfer. Two such relations may be obtained by applying energy balance
(sensible heat relationship) to the hot and cold fluid. Sensible heat expressions might be
obtained by relating total heat transfer rate to the temperature different between the hot and
cold fluids and constant specifíc heats are assumed. These equations are independent of flow
arrangement and heat exchanger type. Therefore, these equations are,
QH = (m)hot (Cp)hot (T)hot [1]

Qc = (m)cold (Cp)cold (T)cold I2]

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An expression may be obtained by relating the total heat transfer rate to the temperature
difference between the hot and cold fluid, where T=Th-Tc. This expression would be an
extension of Newton's law of cooling, with the overall heat transfer coefficient (U) used in place
of the single convection(h) as Q= U A (T) m. The T varies with position in the heat exchanger;
it is necessary to work with a rate equation of the following [4] form,
Where,
(T)m= Log mean temperature difference
Q= Total heat load
A= Total heat transfer area
This equation 3 with equations 1 and 2 would be performed a heat exchanger analysis.
Before this can be done, however, the specific form of (T)m must be establish for the parallel-
flow and counter current-flow heat exchanger.

Q = U A (T)m [3]
1.1 Parallel-Flow and Counterflow Heat Exchanger
According to the Figure 1, the hot and cold fluid temperature distribution associated with a
parallel-flow heat exchanger would be summarized to determine expression for (∆T)m as,
1=Thi-Tci and 2=Tho-Tco
Therefore,

1   2
(T ) m 

ln  1 
 2 

Equation 4 would give the log mean temperature difference (∆T)m.

Equation 4 and equation 3 would be able to determine the rate of heat transfer for parallel
flow.

Tho
Thi
Heat
Exchanger Tco
Tci

Figure 1 : Parallel Flow

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The hot and cold fluid temperature distribution associated with the counter current-flow heat
exchanger in Figure 2 in contrast to the parallel-flow exchanger, therefore, would be
summarized to determine the expression for (∆T)m as,
[5]
Tho
Thi
Heat
Exchanger
Tco Tci

Figure 2 : Counter-current Flow

With 1=Thi-Tco and 2=Tho-Tci

Therefore:

1   2
(T ) m 

ln  1 
 2 
Equation 5 would give the log mean temperature difference (∆T)m. Also this equation and
equation 3 would be able to determine the rate of heat transfer for counter flow.

1.2 Equipment Specification

1.2.1 Shell and Tube Heat Exchanger

The heat exchanger operates with heated water HW (70 °C, 158 °F max) as the heating
medium at the Tube-side and ambient or cold water CW at the Shell-side. The heat exchanger
(HE) can be viewed as a Heater for HW to heat CW OR as a cooler for CW to cool HW. Refer
to the diagram for the schematic set of shell and tube heat exchanger.

1.2.2 Heating Medium HW Tank T1

Heating Medium HW, Heat Exchanger Tube-side

Process Variables Instrumentation

Flowrate, USGPM (Gallon/minute) FI(H)
Pressure, psig, Inlet to Heat PG-H
Exchanger TI1
Temperature, °C, Inlet, tl TI2
Temperature, °C, outlet, t2 DPI

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Pressure Drop, mm Water, DP (Tube)

1.2.3 Cold Water CW Tank T2

Cold Water CW, Heat Exchanger Shell-side

Process Variables Instrumentation

Flowrate, USGPM (Gallon/minute) FI(C)
Pressure, psig, Inlet to Heat PG-C
Exchanger TI3(TI)/TI3
Temperature, °C, Inlet, T1 TI4
Temperature, °C, outlet, T2 DPI
Pressure Drop, mm Water, DP (shell)

2. EXPERIMENT
2.1 Preparation Procedures
Start the following preparation procedures step-by-step.
i. Fill tanks T1 and T2 with water to their maximum level, defined by their overflow drain
pipes(D).
Switch ON the main power supply to Model HE12. The switch is at the front of the
panel/cubicle.
ii. Start-up HW
a) At tank T1, shut fully the discharge valve (HV) but open fully its by-pas valve (BVH).
b) Start the HW pump PH for the water to recirculate around its tank T1, via only BVH.
The suction valve of pump PH must remain open at all times.
c) Switch on the heaters at the front of the panel and allow the water in tank T1 to be
heated to 70oC(see TIC5), which will take about 15-20 minutes. Whilst waiting,
proceed to (iii) below.
iii. CW System : Heat Exchanger Shell Side
Meanwhile get familiar with the equipment, instrumentation, piping system and the various
manual valves. The following preliminary procedures are recommended for familiarization.
a) Check that all the CW pumps (PC1,PC2) by-pass valves (BVC1,BVC2) and discharge
valves (CV1,CV2) are opened. Note that the suction valves of all the pumps (PC1,PC2
and PH)must remain open at all times.

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It is good practice to open the pump manual by-pass valve before starting any pump, to avoid
hydraulic shock and damage to any pipeline equipment downstream.

b) Check that the external water supply to tank T2 is always available but is
automatically shut by the mechanical float-level valve at high level in tank T2.
c) Make sure the CW pumps PC1 and PC2 are OFF. Note that the HW pump PH is still
recirculating HW around its tank T1 via its by-pass valve (BVH), but its discharge
valve (HV) is still fully shut.

REMARKS
Take note of the following Remarks :
- Note that whenever PC1 and PC2 are OFF but the heaters are ON, HV
should be fully shut whilst BVH is fully opened, unless instructed
otherwise. Thus no HW is to circulate to the Heat exchanger when there is
no CW flow through the Heat Exchanger. Instead PH circulates Hw around
tank T1 only, via its by-pass valve BVH.
- Remember to operate only one CW pump to the HEX, the discharge valve
of the other CW pump must be fully shut. Eg, To operate only PC1, CV2
must be fully shut whilst CV1 must be fully opened.

iv. Start-Up CW
- Make sure BVC1, BVC2, the manual by-pass valves of the CW pumps, are fully
opened.
- Switch ON only one CW pump, ie PC1 whose suction is from tank T2.
- Open fully the manual discharge valve CV1 but fully shut BVC1 for maximum
CW flowrate FC to the HEX.
- Note the CW recirculation from PC1 back into tank T2 via the heat exchanger
and its return solenoid valve TSV3A. There will also be recirculation via the pump
by-pass valve BVC1 if it is opened.
- Note the CW flowrate FC at the CW flowmeter, FI(C).

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- To start the T2 back-mixing pump PC2, switch ON PC2 whose suction is from
T2. Open its manual by-pass valve BVC2 fully but shut fully its manual discharge
valve CV2. Back-mixing is to ensure a more uniform temperature inside the CW
tank T2.

2.2 RUN 1
2.2.1 Start-up HW

1. Make sure the hot water tank T1is fílled with water up to its overflow drain pipe level.

2. Shut HW discharge valve but open its manual by-pass valve BVH.

3. Starts pump PH for HW to circulate around tank T1 via only BVH.

4. Start Heaters and note the rise in temperature at tank T1, at TIC5*

5. With BVH fully shut, adjust the HW flowrate to about 10 USGPM (read FI(H)) by regulating
its manual discharge valve HV.

2.2.2 Start-up CW

1. Switch ON both the CW pumps PC1 and PC2. Shut fully BVC1 and CV.

2. Quickly adjust the CW flowrate to about 6 USGPM (read (FI(C)) by regulating only CV1,
the manual discharge valve of the CW pump PC1.

2.2.3 Start RUN I: Taking Reading

1. Refer to Data sheet section. Get ready to collect data for RUN 1.

2.2.4 Pressure drop reading

1. To measure pressure drop in the shell side of the heat exchanger, switch the DP selector
switch to the DP (Shell) position. Take the reading when the reading is steady and within
variation band of 10 - 20 mm H20.

2. After taking the DP (Shell) reading, switch the DP Selector switch to the Equalizing
(Vertical or "O") position to allow the DPI to "Zero" itself before using it again for the next
measurement.

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3. To measure pressure drop in the tube side of the heat exchanger, switch the DP selector
switch to the DP (Tube) position and repeat the same procedure as measuring shell side
pressure drop.

2.2.5 CW and HW Flowrates and Temperatures Reading

1. Take the first set (set 1) of the flowrate and temperature readings for RUN 1:

As the temperature is not steady yet, take the best set of readings possible.

CW : Flowrate FC at FI(C) in USGPM.

Temperature – (Inlet/outlet) : TI3*(T1) and TI*(4)(T2).

HW : Flowrate FH at FI(H) in USGPM.

Temperature-( inlet/outlet) TI1(t1) and TI2(t2).

2. The CW outlet temperature (T2) varies together with the HW inlet/outlet temperatures t1/t2.
It is important to make sure all the temperature readings can be taken simultaneously.

2.2.6 CW and HW Pressure Reading

1. Take the pressure at the pressure gauges PG-C and PG-H.

CW: PG-C, in barg or psig (Assume 1 Bar = 14.5 psi)

HW: PG-H, in barg or psig. (Assume 1 Bar = 14.5 psi)

2. Refer the data sheet for RUN 1. The reading for Set 1, RUN 1 is now completed. Continue
and take Set 2 and Set 3 of the above reading.

2.3 END RUN 1

1. Stop all CW pumps PCl and PC2.
2. Keep the Heaters ON for the next RUN.

3. With the HW pump PH still running, shut fully the discharge valve HV but open fully the by-
pass valve BVH.

4. Make sure the hot water tank T1 is fílled with water up to its overflow drainpipe level.

5. Switch the DP Selector Switch to the Equalizing (Vertical or "O") position.

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2.3.1 Analysis : Heat Balance
Whilst waiting for the HW in tank Tl to be heated to about 70 °C for RUN II, analyze
the data by computing the Qc and QH values for each of the three (3) sets of readings
for the previous RUN 1 as follow:

a) For each Set of reading in RUN I, calculate the heat load Qc and QH for the CW and
the HW as in tutorial.

b) Compare the three (3) calculated values of Qc and QH for RUN I. Select the set of
Qc
readings where  1 . Use the selected set of data to compute the LMTD and the
QH
overall heat transfer coefficient, U.

2.4 RUN II, III and IV

Continue RUN II, III and IV at different flowrates of CW and HW by repeating the procedure
for RUN I.

Suggested Flowrate for RUN I, II, III and IV.

**
RUN HW,FH CW,FC
I 10 USGPM 6 USGPM
II 10 USGPM 10 USGPM
III 15 USGPM 10 USGPM
IV 20 USGPM 10 USGPM

Record all readings in Data Sheet 1 and 2.

3.0 RESULTS AND DISCUSSION

1. Perform mass balance and energy balance on the Shell and Tube Heat Exchanger.

2. Compare the experimental results and predicted results from Microsoft excel.

3. Compare and calculate the values of Qc and QH and select the set of temperature and
flow rates data where calculated values of Qc and QH are close to each other

Note: The Q (total heat load) is approximately equal to the average value
between calculated value Qc and QH.)

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4.0 TUTORIAL
1. Discuss the advantages and disadvantages of using heat exchanger in Oil and gas
processes. Describe an example of industrial applications that utilized heat exchanger
in its process.
2. Write a one-paragraph summary of any journal article that studies on shell and tube
heat exchanger process. The article must have been published within the last 5 years.
Explain on the equipment used in the study and its significance to the study done

REFERENCES
1. Geankoplis C.J. : "Transport Process and Unit Operations", 3rd Edition, Prentice Hall
PTR, 1993
2. J.P. Holman : "Heat Transfer", 7"1 Edition, McGraw Hill, 1992
3. McCabe W.L, Smith J.S. and Harriot. P : " Unit Operation of Chemical Engineering", 5th
Edition, McGraw Hill, 1993.

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EXPERIMENT 5
DISTILLATION PROCESS
OBJECTIVES
To conduct mass balance and energy balance in dIstillation process
To compare the experimental results and the predicted results from
software

Bubble Cap Distillation Process.

1. Introduction.
Distillation is one of the important unit operations in many chemical industries
and has been used from the inception of chemical and process industry.
Distillation is used for the separation of components in a liquid mixture of
volatile constituents. The Distillation Column is usually a vertical column where
the liquid and vapour phases of the mixture are made to mix and approach
equilibrium. The Bubble Cap Distillation Column provides distinct stages at
which such equilibrium can be approached.

Distillation is a process of separating the components of a solution by the

application of heat when the vapour produced by boiling the solution has a
different composition to that of the solution. If the vapour formed is condensed
and subsequently reboiled it will produce, yet again, a vapour of different
composition. Repeated boiling of condensed vapours will ultimately produce a
product of desired quality rich in concentration of one of the components of the
original solution.

Distillation takes place in a Distillation Column which, in essence, comprises a

Boiler, a Column and a Vapour Condensed. The Boiler provides the heat for
vapour generation; within the column rising vapours continually mix with liquid
flowing down the column, condense and are reboiled until vapour of required
composition leaves the column and condenses in the Vapour Condenser to be
removed as Liquid Product. A certain proportion of this condensate is returned
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to the column, called Reflux, the proportion being a major influence on the
quality of the product achieved.

Since this experiment use Batch Distillation plant, therefore, it can be said that
this is a process whereby a specific quantity of a liquid mixture is separated into
its components. The technique is used extensively in laboratories and small
scale production plants where the equipment is often used for separating
several different mixtures of where if only one mixture is separated, the mixture
is not produced continuously. The relatively high capital cost of Continuous
Distillation Plants with their sophisticated control systems, often results in
smaller companies operating Batch Distillation plants. Batch Distillation is
particularly useful for separating liquid mixtures contaminated with solids which
would otherwise foul a continuous plant.

The unit consists of Distillation Column filled with Bubble Cap Trays with a
Vacuum Jacket and Thermo-siphon Boiler, Vapour Condenser, Infinitely Variable
Reflux Control, Distillate Cooler and Receiver, all manufactured in Borosilicate
Glass. Vapour generated in the Reboiler rises through the column and is
condensed in a Vertical Water-Cooled Condenser. The condensed product
leaves the column and passes into an Infinitely Variable Reflux Ratio Controller
incorporating the Variable Area Flow Meters. Each column component has five
Bubble Cap plates with a temperature measurement nozzle on each plate.
Vapour and liquid compositions throughout are determined by respective
temperatures. The unit is equipped with the facility for liquid and gas sampling at
the top and bottom of the column. A Condenser consists of a coil type Heat
Exchanger. A Reflux Separator is provided at the top of the column. Reflux is
returned to the column and the product passes through a cooler and a graduated
pipe section and can be passed either to a receiving vessel, which allows
product removal while operating under vacuum or back to the Boiler.

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A sketch of a tray with Bubble Caps is as shown in the diagram below.

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2. Chemicals and Ancillary Equipments Required :

a.) Chemicals Required.
• Ethanol industrial grade.
• Water

b.) Ancillary Equipments Required :

• Two 2000ml beakers and two 250ml beakers.
• Refractometer for measurement of sample concentrations.
• Calibration Curve for the Refractive Index Vs Concentration of Ethanol
Water mixtures.

3. Operating Instructions.
3.1 Safety Considerations.
• You must familiarize yourself with each item such as the Reboiler,
Condenser, Distillation Unit and the flow paths and apparatus before
conducting of the experiment. This distillation operation usually deals
with very hot and highly flammable materials. Extreme care must be
taken when handling the apparatus, in taking readings and collecting
samples.
• The Flow Meters should be operated smoothly in order to avoid pressure
surges within the equipment.
• Inspect the equipment visually for any damaged components or glass
breakage. If any such defects are noticed, please report them to your
instructor / technician.
• Goggles must be worn at all times in the laboratory.
• Appropriate rubber gloves must be worn when Organic Solvents are
handled.
• Avoid wearing clothes which can easily catch fire.
• The flow rates of liquids should not exceed the maximum of the rates
shown in the flow meter.
• The water supply pressure to the Condenser and the Coolers should not
exceed 2 bar gauge.

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• Inspect the equipment visually for glass breakage and leakage.

• Replace any defective items in accordance with the CTS2.
• Do not allow the water pressure to exceed 2.0 bar maximum as indicated
by PI.2.
• Always maintain V.8 in the open position during atmospheric operation
(avoid system pressurizing).
• Don’t isolate cooling water until the heating has been shut down (at
least 10 minutes ).
• Don’t switch on the immersion heater with the level in the reboiler below
the heater elements or when the reboiler is empty.
• Don’t return the product distillate collected to the reboiler vessel
when the equipment is in operation.
• Do not allow the liquid level to rise much above the top graduation on
the tube before the stop valves V.2 and V.3 are opened.
• Don’t drain the liquid in reboiler vessel until is cold.
• Do not touch the hot components of the unit.

3.2 General Start-up Procedures.

Materials needed :
a.) Ethanol industrial grade.
b.) Water

• Prepare between 30 to 40 litres of 10 % to 20 % mixture of Ethanol in

Water by mixing appropriate quantities of the Industrial Grade of
Ethanol in Distilled Water.
• Ensure valves V.1, RCV.1, V.3, V.4, V.5, V.6, V.7, V.9 and FCV.2 are
closed.
• Ensure valves V.2, V.8 and V.10 are open.
• Slowly open the cooling water to the condenser (max 2.0 bar).
• Make sure water is indeed flowing through it.
• Check water flows to the drain from the Cooling Water outlets.

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• Do not start the experiment until the Cooling Water flow is visible in the
outlets to the drain.
• Ensure that the Bottom Product and Top Product sampling valve is closed.
• Ensure that the Reboiler Vessel is already charged with the Ethanol –
Water mixture through the Charge Port ( Refer to the diagram ).
• Check that the liquid level is satisfactory ( Refer to instructor / technician ).
• Otherwise top up with the Ethanol – Water mixture through the Charge Port
( Refer to instructor / technician ).
• Ensure that the concentration of feed in the reboiler vessel is correct and
that the liquid level is at the vessel equator.
• The Reboiler Vessel should never be filled with liquid above the maximum
level indicated.
• The level should never recede below the minimum level while on operation.
• Close the Reflux Adjustment Valve and valve below Product Cooler.
• Obtain a sample of Ethanol – Water mixture from the Reboiler through
the Sampling Port and test its composition using Refractometer and
given graph of Refractive Index Vs Mole Fraction of Ethanol in Liquid.
• Turn on the main power control switch.
• Turn on the power switch of the heater.
• Switch on electrical supply (green ‘heater on’ button).
• Set heater controller HC.4 to maximum setting.
• When distillate liquid is seen to flow through RI.A1, reduce the heat input
and set HC.4 to give an RI.1A reading of 7.5.
• Allow a period of 15 minutes for the equipment to maintain thermal
equilibrium with surroundings.
• During this period continue to adjust HC.4 to maintain a reading of 7.5
on the reflux rotameter RI.1A.
• The unit is now ready to be used for an experiment.

3.3 Experiment : Operation Under Partial Reflux Conditions.

Procedure :
• Ensure that the valve for Reflux Ratio adjustment are opened.
• Adjust both valve for Reflux Ratio and valve below Product Cooler so that

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both readings on R1 and R2 provide a Reflux Ratio of 1.0 for the
operation.
• Wait for about 15 minutes until the flow rate shown by R1 and the
temperature readings at the top and bottom of the columns are steady. (
Refer to instructor / technician ).
• Collect samples from the Reboiler and the overhead from the Sampling
Port for every 5 minutes.
• Observe the flow rate at R1. Adjust the valve for Reflux Ratio
adjustment to ensure that the Reflux Ratio is maintained at 1.0.
• The concentration of the samples drawn is measured using the
Refractive Index method.
• Record the reading of temperatures for every 5 minutes.
• Readings are recorded in the provided table of results.

3.4 General Shut – Down Procedures.

 Switch off electrical supply (red ‘heater off’ button).

 Turn off the power switch of the reboiler.
 Adjust heater controller HC.4 to minimum setting.
 Turn off the main power control switch.
 Do not drain the hot liquid from the Reboiler. If necessary, the liquid within
the system could be drained only when the liquid is already cooled.

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Time Temperature Readings ( º C ) RI RI
(Min) TI 1 TI TI TI 2 TI TI TI 4 TI 5 TI 6 Top Bottom
1A 1B 2A 2B Product Product
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85

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RESULT AND DISCUSSION

1. By using the temperature of reboiler an condensate, determine ethanol
concentrations in bottom and top product and compare with your result
( use boiling point diagram)
2. Perform mass balance and energy balance on distillation process.
3. Compare the experimental results and predicted results from Microsoft
excel or software
4. Discuss the effect of the reflux ratio in distillation column and how the
changing the reflux ratio affected your result

TUTORIAL
1. Describe an example of industrial applications that utilized distillation in its
process. Discuss the advantages and disadvantages of using bubble cap
distillation process in chemical plant.
2. Write a one-paragraph summary of any journal article that studies
distillation process. The article must have been published within the last 5 years.
Explain on the distillation process type used in the study and its significance to
the study done.

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