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MASS TRANSFER (EP203)

LABORATORY MANUAL

Lecturer/Instructor: _______________________________

Name

:____________________________

Student ID

:____________________________

Course

:____________________________

FACULTY OF ENGINEERING, ARTCHITECTURE &


BUILT ENVIRONMENT
UCSI UNIVERSITY
2016

TABLE OF CONTENT

General Instructions
General Techniques

Preparation of a Refractive Index (RI) vs Composition Plot

Experiment 1

Batch Distillation at Total Reflux

Experiment 2

Batch Distillation at Constant Reflux

Experiment 3

Absorption of Carbon Dioxide From Air Into Water

Experiment 4

Absorption of Carbon Dioxide From Air Into Sodium


Hydroxide

Experiment 5

Studies on Drying Characteristic of Fruitsby Using Different


Drying Methods (OPEN ENDED)

APPENDIX
1

Distillation Column

Absorption Column

Example of Front Page

Example of Cover Page

Reference Citing Method

GENERAL INSTRUCTIONS

The experiments in this manual are designed to give engineering students an


introduction to material science including aspects such as atomic structure, material
properties and testing. These experiments are also intended to teach students the
principles of laboratory protocol and reporting.

Students are required to carry out all the experiments following the general
methods and procedures presented in this manual. All experiments are to be completed
within the allotted time. Students are expected to be prepared prior to coming for the
laboratory session. This includes reading the lab procedure thoroughly and understanding
the objectives, operations and hazards that may be encountered during the experiment.

The laboratory experiments shall be conducted in groups. Thus, students have to


learn to organize themselves within the groups and to allocate responsibilities among
themselves.

LABORATORY PROCEDURE AND CONTROL

2.1 Logbook

You are required to keep a logbook for experiments. This must be a bound logbook.
You are required to translate the procedure of each experiment in the laboratory manual
into graphical illustrations or a flowchart in your logbook before you start.

Record in your logbook every action and observation as you carry out the experiment.
Records should be as brief, but concise, as possible.

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. Clarity of procedure and results are important. Always
use a pen to write on your logbook. Mistakes made should be crossed out clearly. Use of
liquid paper or eraser is not allowed.

The lab instructor/lecturer will inspect and sign your logbook during the lab
session and possibly grade them at the end of the semester.

2.2 Laboratory group

You will be assigned into a 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 groups. You are required to work with your group members as much as
possible in terms of understanding the experiment and sharing information on the
different activities performed by different members. At the end of each of the session,
each of the group members is required to carry out peer evaluation. Peer evaluation is
private and confidential. The purpose of peer evaluation is to ensure that all group
members contribute throughout the laboratory session.

2.3 Laboratory Reports

Each student will be responsible for preparing an individual report


aftercompleting each laboratory experiment.

(a)

Report submission
Reports must be submitted one (1) week after the scheduled experiment and
within the first ten (10) minutes of the due lab period. Any unforeseen
circumstances must be reported to the lab instructor immediately. Late
submissions will not be accepted.

(b)

Report style/format
Reports may be typed-written. Type written text shall be spaced, using font type
New Times Roman and font size 12. It is recommended that an equation editor be
used. Atomic structures and other figures may be drawn by hand.

The report shall be:


(i)

Written in the passive tense. Example: Five milligrams of solid was


weighed.

(ii)

Graphs must be complete with title, axis labels with units and legend
where necessary. The scale of the graph should be appropriate for the data
obtained.

(iii)

(c)

PLAGIARISM WILL NOT BE TOLERATED.

Report contents
Each report should contain the following:
(i)

Front page (Refer to Appendix A)

(ii)

Table of contents (Refer to Appendix B)

(iii)

Introduction/background of the experiment


Contains a summary of the experiment that is carried out. This section
includes the statement of purpose or objectives of the experiment and an
introduction to the technique used. It is not necessary to include a
discussion of the basic theory relevant to the experiment. The introduction
of the report should not be more than 20% of the overall report.

(iv)

Material and Methodology


This is a brief description of the experimental approach used. It should
include a brief description of the test apparatus and instrumentation used,
as well as the procedure used to obtain the test results. Summarize the
detailed steps used; do not repeat the steps given in your lab experiment.

(v)

Results and discussion


Test results obtained from the experiment shall be presented in the
applicable format: Narrative, tabular, graphical, photographic, or a
combination of the above. Numerical data must be presented realistically
with appropriate number of decimal places. Data should be tabulated
neatly showing raw experimental data, if necessary, and reduced (useful)
data.
Calculations for reduced data should be briefly described and need not be
worked out. Identify formulas, charts, tables or handbooks that were used
to obtain the final result. If needed, you may refer sample calculations to
the appendix. Any questions given in the lab sheet should be answered in
the Discussion section.

(vi)

Conclusion
This section summarizes your findings of the experiment. If results differ
from those expected, provide an explanation based on an analysis of the
data. Examine any assumptions used that could be adversely affecting the
results.

(vii)

Limitation of the Experiment/Difficulties Encountered (if any)


Consider any limitations or difficulties encountered during the experiment.
Include also any errors that may have occurred. Suggest ways for
improvement.

(viii)

Reference
A minimum of three (3) references should be cited in your report. Refer to
Appendix C for the format of citations.

(ix)

Appendix (if any)

2.4 Assessment

The laboratory component accounts for 10% of the total marks for the subject.

Marks for each report shall be allocated as follows:

Items
Score

Unacceptable
1

Satisfactory
2

Good
3

Excellent
4

Objective are
irrelevant or are not
appropriate to the
experiment

Objective /
introduction miss at
least one important
consideration

Introduction and
objective are listed,
important
experimental details
are covered, some
minor details missing

Introduction and
objectives fully
addressed.

Timeliness

Report handed in
more
than two days late

Up to one day late

Up to one hour late

Report handed in time

Experimental
procedures

Procedures do not
accurately list the
steps of the
experiment

Procedures are listed,


but seem missing
some information,
some steps are not
numbered and/or are
in incomplete
sentences.

Procedures are listed,


important
experimental details
are covered, some
minor details missing

Procedures are listed in


clear steps; each step
is numbered and in a
complete sentence.

Result: data,
figures,
graphs,
tables, etc.

Figures, graphs,
tables contain
errors or are poorly
constructed, have
missing titles,
captions or
numbers, units
missing or
incorrect, etc.

Most figures, graphs,


tables OK, some still
missing some
important or required
features

All figures, graphs,


tables are correctly
drawn, but some have
minor problems or
could still be improved

All figures, graphs,


tables are correctly
drawn, are numbered
and contain
titles/captions.

Discussion/
Observation

Very incomplete or
incorrect
interpretation of
trends and
comparison of data
indicating a lack of
understanding of
results

Some of the results


have been correctly
interpreted and
discussed; partial but
incomplete
understanding of
results is still evident

Almost all of the


results have been
correctly interpreted
and discussed, only
minor improvements
are needed

All important trends and


data comparisons have
been interpreted
correctly and
discussed, good
understanding of
results is conveyed

Conclusion

Conclusions
missing or missing
the important points

Conclusions
regarding major
points are drawn, but
many are misstated,
indicating a lack of
understanding

All important
conclusions have
been drawn, could be
better stated

All important
conclusions have been
clearly made, student
shows good
understanding

Appearance
and
formatting

Sections out of
order, report is not
typed/written using
the appropriate
format

Sections in order,
formatting is rough
but readable

Lab report is mostly


typed/written using
the appropriate
format, all sections in
order, formatting
generally good but
could still be improved

Lab report is
typed/written
in well-formatted, very
readable.

Spelling,
grammar,
sentence
structure

Frequent grammar
and/or spelling
errors, writing style
is rough and
immature

Occasional
grammar/spelling
errors, generally
readable with some
rough spots in writing
style

Less than 3
grammar/spelling
errors, mature,
readable style

All grammar/spelling
correct and very wellwritten

Objective
and
Introduction

Total Mark
Final Score
Percentage (%)

= (Total Marks / 32
)*10

Score

Laboratory Safety

All safety requirements as specified in this section will be strictly enforced.


Students are required to comply with the following rules when in the lab.

1.

Wear closed shoes and lab coats at all times while in the laboratory. Eye
protection (goggles) should be used when necessary.

2.

Wear suitable attire for lab work. Do not wear loose or bulky clothes, ties or
jewelry when working around rotating equipment. Students with long hair must tie
their hair before entering the lab. Open-toe shoes and sandals are not
permitted. (Lecturer/instructor reserves the right not to allow students who do
not follow this rule to enter the lab).

3.

Eating and drinking in the lab are strictly prohibited.

4.

All hand phones must be switched off.

5.

Always be punctual. Students later than 15 minutes are not allowed to


perform the experiment.

6.

Students must have a towel (for cleaning purposes), a logbook and their lab
manual during the lab session.

7.

Always follow the instruction of the lab instructor or lecturer before the start
of the lab.

8.

Clean the bench and return all apparatus to their respective places before you
leave the lab. (otherwise each of member in you group marks you, will be
deducted)

9.

Use only required amounts of reagents to avoid wastage and excess.

10.

Dispose of excess reagents as instructed, never return excess reagents into the
bottle. Some used chemicals may be washed down the drain, while others
require a different method of disposal. If a chemical can go in the sink, be sure to
wash it away thoroughly rather than risk an unexpected reaction between chemical
leftovers later.

11.

Make sure you know the location of the following safety devices: eyewash station,
emergency shower, fire extinguisher, fire alarm station, emergency evacuation
route.

12.

Handle all equipment with care to avoid damage during experimental operations.

13.

Clean up broken glass and report to the lab instructor or lecturer immediately.

PREPARATION OF A REFRACTIVE INDEX (RI) VS. COMPOSITION


PLOT
1. Prepare a set of mixtures containing ethanol and water within a specified range of
composition between pure water and pure ethanol as following table :

Table 2: Composition Data Based on Refractive Index


Volume
of
ethanol
(ml)

Volume of
water (ml)

10

1.0

9.0

2.0

8.0

3.0

7.0

4.0

6.0

5.0

5.0

6.0

4.0

7.0

3.0

8.0

2.0

8.5

1.5

9.0

1.0

9.5

0.5

10.0

0.0

Mole
fraction
ethanol

Ethanol
Wt%

Mass of
ethanol (g)

Mass of
water
(g)

Refractive
Index (RI)

2.

For each mixture, obtain their refractive index (RI) readings using a refractometer.

3.

Prepare a plot of refractive index (RI) vs. ethanol mol fraction for the whole range
of mixtures. This will serve as the calibration curve for further experiments.

EXPERIMENT 1: BATCH DISTILLATION AT TOTAL REFLUX


OBJECTIVE:

To determine the height equivalent theoretical plates (HETP) at total reflux.


To determine the effect of liquid and vapor loading on the HETP at total reflux.
PROCEDURES:

1.

Perform the general start-up procedures (Section 4). Refer appendix 1.

2.

Set heater power control to 1.0 kW and allow the reboiler temperature reach
approximate 85oC.

3.

Ensure the reflux control is 1 position. (total reflux)

4.

As the top column temperature sensor TT 112, reach steady state, record the
temperature.

5.

Measure the distillate flow rate as follows:


a)

Set the reflux control to position 1(Total reflux)

b)

when the distillate start flowing into the phase separator, start the timer.

c)

As distillate reach 200 ml on the measure tank(overflow), stop the timer.

d)

Determine the flow rate of the distillate.

6.

Set the reflux control to position 2 (Total distillate offtake). Open valve V9 and
collect 10 ml sample distillate using conical flask. Close valve V9 and set the
reflux control to position 1. ( Total reflux).
7. To collect bottom product sample, adjust the overflow U-tube to a
suitable level to let the product overflow into the product tank, B5 after
passing through the product cooler, W3. Open valve V2 and V3 and
collect 10 ml of sample bottom product using conical flask.Close valve
V2 and V3.
8. Measure the refractive index of the samples and record the value into
data table.
9. Wait for approximately 15 to 30 minutes and allow the distillation unit
to achieve new steady state.
10. Repeat steps 2 to 8 for different liquid and vapor loading, adjust the
heater power settings according table below:
Heater Power
(kW)
1.00
1.50
2.00

ANALYSIS & DISCUSSION:


1. Use the sample table in Appendix 1 for data collection.
2. Using the X-Y equilibrium diagram for ethanol-water system, mark the
top and bottom compositions on the diagram and determine the
theoretical number of plates in the distillation unit using the McCabeThiele method.
3. Calculate the height equivalent theoretical plates (HETP) by dividing
the effective column height with the number of theoretical plates.
4. Plot a graph of HETP vs. Heating Power and observe the relationship.

EXPERIMENT 2: BATCH DISTILLATION AT CONSTANT


REFLUX
OBJECTIVE:

To operate a batch distillation unit at constant reflux.


To examine the change in top and bottom composition over time in a
batch distillation.

PROCEDURES:
1. Perform the general start-up procedures (Section 4). Refer appendix 1.
2. Record initial volume and refractive index of the liquid mixture in the
reboiler.
3. Set the heater power to 1.5kW.
4. Set reflux timer to 10 second for set 1 and 30 second for set 2.
( Note: Set 1: Product liquid to tank B4 (distillate) ; Set 2: Product
liquid return to column (reflux)).
Set the reflux control to position 3. (Timer controlled reflux).
5. As the top column temperature sensor, TT 112 reach steady state,
record the temperature.
6. Open sampling valve V9 and collect 10ml of distillate sample using
conical flask. Close valve V9.
7. Adjust bottom overflow level. Open valve V2 and V3 and collect 10
ml of sample bottom product using conical flask.Close valve V2 and
V3.
8. Measure the refractive index of the samples and record the value into
data table.
(Note: Do not discard the sample as to perform material balance at
the end of the experiment.)
9.

Repeat steps 6 to 9 until the bottom sample RI values constant.

10. Switch off heater power and allow the system to cool down to ambient
temperature.
Optional Mass Balance Calculation:
11. Open drain valve V12 and collect all the liquid from the reboiler.
Measure the volume and refractive index of the liquid. Record all the
values.
12. Open valve V7 and collect all the distillate from product tank. Measure
the volume and refractive index of the distillate. Record all the values.
(Note: Remember to include all previous samples.)

ANALYSIS & DISCUSSION:


1. Use the sample table in Appendix 1b for data collection.
2. Compare the quality of distillate among the sieve tray column and the
packed column.
3. Using the X-Y equilibrium diagram for ethanol-water system, mark the
top and bottom compositions for each sampling time on the diagram.
Observe the change of composition over time in the batch distillation
column.
4. Plot graph of composition vs time and temperature vs time.

EXPERIMENT 3: ABSORPTION OF CARBON DIOXIDE FROM


AIR INTO WATER

OBJECTIVE:

To demonstrate the absorption of CO2 into water using a packed


column.

To calculate the rate of absorption of CO2 into water.

To determine the saturation composition of CO2 in water.

To study the effect of gas flow rate, gas inlet composition and
liquid flow rate on the rate of CO2 absorption.

PROCEDURES:
1.

Perform the general start-up procedures as described in Section 4


(refer appendix 2).

2.

Fill the sump tank B1 with up to 40-L of fresh water. Open valve
V4.

3.

Switch on circulation pump P1 and allow the water to bypass into


the sump tank B1 via valve V4.

4.

Introduce air and CO2 mixtures into the absorption column K1 as


follows:
i. Determine the appropriate air and CO2 gas flow rate in order
to achieve the desired inlet gas composition for the absorption
process.
ii. Open and adjust valve V1 to set the flow rate of gas CO2, FI101.
iii. Open and adjust valve V2 to set the flow rate of air, FI-102

5.

Record the initial CO2 concentration in the sump tank B1 as the


feed composition value.

6.

Introduce liquid into the absorption column K1 as follows:


i. Slowly open valve V3.
ii. Observe liquid entering the top of the absorption column,
flowing down the column and back into the sump tank B1.

iii. Adjust valve V3 to fix the desired inlet liquid flow rate at FI103
7.

At regular intervals of 5 minutes, collect a sample from the outlet


liquid of the absorption column K1 as described in Section 4.4.
Analyze the collected sample to determine the concentration of
dissolved CO2 in water (Section 4.5).

8.

Continue to record data and collect liquid and gas samples until the
CO2 composition in the sump tank B1 and the outlet gas has
reached a steady value.

9.

Stop the experiment and perform the general shut-down procedures


as described in Section 4.3.

10. Repeat the experiment by changing the gas flow rate, gas inlet
composition and liquid flow rate.

RECOMMENDATIONS:
Variables

Range

Air flow rate

40 L/min

CO2 gas flow rate

4-8 L/min

Inlet gas composition

9-16 vol%

Liquid flow rate

4.0 L/min

ANALYSIS & DISCUSSION:


1. Use the sample table in Appendix 2 (table 2A) for data collection.
2. Plot the CO2 composition in the inlet water flow as a function of time.
3. Compare the CO2 composition plots for different gas flow rates, gas
inlet compositions and liquid flow rates.

EXPERIMENT 4: ABSORPTION OF CARBON DIOXIDE FROM


AIR INTO NaOH
OBJECTIVE:

To demonstrate the absorption of CO2 into NaOH using a packed column


To calculate the rate of absorption into NAOH
To determine the saturation composition of CO2 in NaOH
To study the effect of gas flow rate, gas inlet composition and liquid flow
rate on the rate of CO2 absorption.

PROCEDURES:
1.

Perform the general start-up procedures as described in Section 4.2.


(refer appendix 2)
2. Fill the sump tank B with up to 40-L of NaOH 0.1M. Open valve V4.
3. Switch on circulation pump P1 and allow the NaOH to bypass into the
sump tank B1 via valve V4.
4. Introduce air and CO2 mixtures into the absorption column K1 as follows:
I. Determine the appropriate air and CO2 gas flow rate in order to
achieve the desired inlet gas composition for the absorption process.
II. Open and adjust valve V1 to set the flow rate of gas CO2, FT-101.
III. Open and adjust valve V2 to set the flow rate of air FT-102.
5. Record the initial CO2 concentration in the sump tank B1 as the feed
composition value.
6. Introduce liquid into the absorption column K1 as follows:
I. Slowly open valve V3.
II. Observe liquid entering the top of the absorption column, flowing
down the column and back into the sump tank B1.
III. Adjust valve V3 to fix the desired inlet liquid flow rate at FT-103.
7. At regular intervals of 5 minutes, collect a sample from the outlet liquid of
the absorption column K1 as described in Section 4.4. Analyze the
collected sample to determine the concentration of dissolved CO2 (section
4.5).
8. Continue to record data and collect liquid samples until the CO2
composition in the sump tank B1 has reached a steady value.
9. Stop the experiment and perform the general shut-down procedures as
described in section 4.3 (refer appendix 2).
10. Repeat the experiment by changing the gas flow rate, gas inlet composition
and liquid flow rate.

REMARK:
Procedure to clean the equipment after the usage of NaOH
I.
II.
III.
IV.

V.
VI.
VII.
VIII.

IX.

Drain all of the NaOH from the equipment by opening valves V3,
V4, V5, V6 and V7.
After draining, close valve V7.
Fill the sump tank with 20L of 0.1M HCl.
Switch on the pump P1 and circulate the HCl solution in the
equipment. Open valve V3 to the maximum. Let the fresh HCl
circulate for around 10 minutes.
Drain all of the HCl by opening valves V3, V4, V5, V6 and V7.
After draining, close valve V7.
Fill the sump tank with 40L of fresh water.
Switch on the pump P1 and circulate the fresh water in the
equipment. Open valve V3 to the maximum. Let the fresh water
circulate for around 10 minutes.
Cleaning process completed. Drain all of the HCl by opening
valves V3, V4, V5, V6 and V7.

RECOMMENDATIONS:

Variables

Range

Air flow rate

40 L/min

CO2 gas flow rate

2-5 L/min

Inlet gas composition

4.76-11.11 vol%

Liquid flow rate

2.0 L/min

ANALYSIS AND DISCUSSION:

1. Use the sample table in appendix A for data collection


2. Plot the CO2 composition in the inlet NaOH flow as a function of time.
3. Compare the CO2 composition plots for different gas flow rate, gas inlet
compositions and liquid flow rates.

EXPERIMENT 5: STUDIES ON DRYING CHARACTERISTIC OF


FRUITS BY USING DIFFERENT DRYING METHODS
(OPEN ENDED EXPERIMENT)
The most effective way to dry any fruits or vegetables (or even meats) is to expose
them to heated air. This will remove moisture and leave behind the solids and materials
which were previously dissolved in the water. Sources of heat can include burning
various fuels, or other more environmentally friendly methods such as sun-drying.
ProposeTWO different techniques of drying to determine below analysis and compare the
result for each drying techniques.You may choose any types of fruits.
1) Determination of rehydration ratio
2) Determination of moisture content
In the report, students are required to include details of:
1)
2)
3)
4)

What happens in the drying process


Factors affecting drying
The role of air temperature
How do drying methods compare

Make sure that you identify all possible hazards associated with any chemicals or
apparatus that you use and understand the correct procedures for disposal of any waste
chemicals.
Present your results as a written report in which you provide full details of the procedure
and discuss the differences observed in the characteristics of each analysis.

APPENDIX 1 (DISTILLATION COLUMN)

CW

V1
W2

B6

Condenser
0.5m2

Dosing tank
5-L

Vent /
Vacuum

B7
Phase separator

FI

TT

102

112

KS 01

V10
V-1

TT 101
TT 102
TT 103
TT 104
TT 105

V9

V11
B4
Packed Column, K2

TT 106
TT 107
TT 108
TT 109
TT 110

DN50 x 1.0m
8mm Raschig ring

TT

FI

FT

111

101

101

Distillate
Product tank
5-L

DPT
301

V7
V-2
V13

TIC

V5

W3

LS
01

Product Cooler

P1

B1

DN50 x 1.0m

Metering
pump
12 L/hr

CW
W1a, W1b
Immersion
heater Reboiler
7-L
2 x 1kW

B3
Feed tank
5-L

V4

201

Sieve Tray Column, K1

B2
Feed tank
5-L

V8
B5

V2
V12

Bottom
Product tank
5-L

V3

Figure 1: Process flow diagram of continuous distillation column

V6

SECT 4: GENERAL START-UP PROCEDURE FOR DISTILLATION COLUMN

4.1

Set the Timer Controlled Reflux (KS-01)

1. The Distillation Column Unit, BP 80-50 can be running in total reflux mode
and different reflux ratio mode.
2. The MODE button is for the selection among Set 1 and Set 2 timer setting.
Set 1 is the time for the distillate to flow into the product tank, B4. Wheres
Set 2 is the time for the distillate to flow back into the distillation column, K1
and K2.
3. To set the desired time value, follow the below steps:
(a) Press the MODE button to select the desired Set of time.
(b) Use the arrow button to choose the position of the figure which we want
to set the value.
(c) At the desired position of the figure, press the + button to set the
desired value.
Note: The + button can only increase the value in one way, which is a
circulation from 0 up to 9.
(d) After the desired value is set, press the ENT button to end the time
setting.

4. Instruction for the reflux controller, KS 01 on the control panel:


(a) Position 1: Total reflux
(b) Position 2: Total distillate
(c) Position 3: Timer controlled reflux.

4.2

General Start-Up Procedures

1. Ensure all valves are closed.


2. Prepare a mixture of ethanol and water at desired composition (for
instance 5 L mixture containing 2 L of ethanol and 3 L of filtered
water). Open the charge port cap and charge the reboiler B1 with the
ethanol-water mixture. Close the charge port cap.
(Note: You can use any suitable binary system other than ethanol
water.)
3. Prepare another mixture of ethanol and water (4 L of pure ethanol and
6 L of filtered water) and pour into feed tanks B2 and B3 separately.
4. Make sure all the valve are properly close except V4, V5, V1, and V8.
5. Turn on the main power on the control panel.
6. Set the reflux divider to 1 position (total reflux). This is to prevent any
distillate from escaping when start up the distillation unit.
7. Open the main cooling water valve V1. Let the cooling water flow into
the condenser (W2).
8. Switch on the cartridge heaters W1a & W1b and set the heater power
controller to 1.0 kW.
8. Allow the liquid in the reboiler to boil. As the liquid boils, the liquid
level in the
reboiler will start to drop.
9. Observe the vapor rising from the boiling liquid into the distillation
column. As
the vapor reaches the condenser, it will condense and flow back into
the column as liquid. Mass transfer will take place between this liquid
and vapor phase in the column.
10. Check that the condenser has sufficient cooling water flow to minimize
escape of vapor into the vent.

11. Let the distillation column run until a stable condition is observed. The
stable condition is reached when all temperature indicators on the
column give a constant reading with an allowable 0.2C fluctuation.
12.

4.3

The unit now is ready for experiment

General Shut-Down Procedures

1. Set the reflux divider to 1 position. (total reflux)


2. Keep the cooling water running through the condenser (W2).
3. Switch off the heater power. Monitor the temperature drop in the
reboiler. Wait until it has cooled down to room temperature.
4. Drain all liquid from the reboiler B1 and product tank B4 and B5.
5. Close the cooling water valves V1 and V8.
6. Turn off the main power on the control panel.

1a) Equilibrium Data for Ethanol-Water System at 1 atm

Table 1: Equilibrium Data for Ethanol-Water System at 1 atm

Temperature
(C)

Mole fraction ethanol


Liquid phase

Vapor phase

100

0.0000

0.0000

95.5

0.0190

0.1700

89.0

0.0721

0.3891

86.7

0.0996

0.4375

85.3

0.1238

0.4704

84.1

0.1661

0.5089

82.7

0.2337

0.5445

82.3

0.2608

0.5580

81.5

0.3273

0.5826

80.7

0.3965

0.6122

79.8

0.5079

0.6564

79.7

0.5198

0.6599

79.3

0.5732

0.6841

78.7

0.6763

0.7385

78.4

0.7472

0.7815

78.2

0.8943

0.8943

(Source: Perrys Chemical Engineers Handbook, Table 13-1, pg. 13-12)

X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm

1.0000

0.9000

0.8000

Vapor mol fraction

0.7000

0.6000

0.5000

0.4000

0.3000

0.2000

0.1000

0.0000
0.0000

0.1000

0.2000

0.3000

0.4000

0.5000

0.6000

0.7000

Liquid mol fraction

Figure 2: X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm

0.8000

0.9000

1.0000

Table 2: HETP
Heater W1a

Distillate

Bottom Product

and W1b

HETP
(mm)

power (1kW)
Temp

Refr.

Mole

Temp

Refr.

Mole

(C)

Index

Fraction

(C)

Index

Fraction

(RI)

(RI)

1.00
1.50
2.00

1b) Table of result for experiment 2


Heater power :
Reflux ratio:
Time (min)

Distillate
Temp (C)

Refr. index

Bottom product
Mole fract.

Temp (C)

Refr. index

Mole
fract.

0
10
20
30
40
50
60

APPENDIX 2 (GAS ABSORPTION)

Figure 1: process flow diagram for the gas absorption unit

Section 4: OPERATING PROCEDURES

4.1

General Operating Procedures

It is important that the user read and fully understand all the instructions and
precautions stated in the manufacturer's manuals supplied with the equipment
prior to operation. The following procedures will serve as a quick reference
for operating the unit.

1. Gas flow rate control


Use the needle valves V1 and V2 to manually control the CO2 and air flow
rates, and consequently the CO2 composition entering the absorption
column K1.

2. Liquid flow rate control


Use valve V3 to manually adjust the liquid flow rate entering the
absorption column. The valve should be closed when the pump P1 is
initially switched on to prevent liquid surge through the flowmeter FT-03

3. Column pressure drop measurements


If the pressure drop readings are fluctuating or inaccurate, liquid may have
been trapped in the tubing leading to the manometer. Remove the tubing
from the manometer side and blow into them to clear off any trapped
liquid along the lines. The air trapped in the tubing also contributes to
inaccuracy of measurement.

4.2

General Start-Up Procedures

1. Ensure all valves are initially closed.


2. Check that all gas connections are properly fitted.
3. Switch on the air compressor and allow the pressure to build up until 5 bar.
4. Open the valve at the CO2 compressor. Set the supply pressure to between
4 to 5 bars by turning the air filter regulator knob clockwise.
5. Open the valve at the air gas supply. Set the supply pressure to between 2
to 3 bars by turning the gas regulator knob clockwise.
6. The unit is now ready for experiments.

4.3

General Shut-Down Procedures

1. Switch off the circulation pumps P1 and air compressor.

2. Close valves V1, V2 and V3.


3. Close the valve on the air compressor and release the supply pressure by
turning the air filter regulator knob counterclockwise all the way.
4. Close the valve at the CO2 gas supply and release the supply pressure by
turning the gas regulator knob counterclockwise all the way.
5. Drain all liquid in the column K1 by opening valve V5.
6. Drain all liquid from the sump tanks B1 by opening valves V7.

4.4

Liquid Sampling Procedures

Samples can be taken from the liquid in the sump tank B1 for analysis. The
sampling valve is located at V7 for inlet liquid to absorption column K1.

The procedures for collecting a sample are as follows:

(i) Place a vial below the sampling valve.


(ii) Open sampling valve and collect the residual water inside the pipeline and
return it to the sump tank.
(iii) Collect about 150 mL of sample using vial.
(iv) Close the sampling valve.
(v) Use pipette to collect 100ml of sample from the sample collected and analyze
the acidity of sample using method described in section 4.5.

4.5

Analysis of Dissolved CO2 in Water

Water for absorption experiment should be deionised because presence of


dissolved salts could affect the analysis method as described below.

CHEMICALS NEEDED:
a) deionised and CO2 free water
b) Phenolphthalein indicator (AR grade)
c) 1.0 L of standard 0.05 M sodium hydroxide (NaOH) solution

PROCEDURES:
1. Obtain a sample as in Section 4.4.
2. Prepare exactly 100 mL of sample in a conical flask.
3. Add 510 drops of phenolphthalein indicator. If the sample turns red
immediately, no free CO2 is present. If the sample remains colorless, titrate
with the standard 0.05 M NaOH solution.

4. Measure the volume of 0.05 M NaOH required reaching the end point. The
end point occurs when a definite pink colour persists in the solution for
longer than 30 seconds.
5. For best results, use a colour comparison standard. Prepare exactly 100 mL
of 0.01 M NAHCO3 solution in a conical flask and add 5-10 drops of
phenolphthalein indicator.
4.6

Analysis of Dissolved CO2 in NaOH


Water for absorption experiment should be deionised because presence of
dissolved salts could affect the analysis method as described below.

CHEMICALS NEEDED:
a) Deionised and CO2 free water
b) Phenolphthalein indicator (AR grade)
c) 1.0L of standard 0.10M sodium hydroxide (NaOH) solution
d) 1.0L of standard 0.10M hydrochloric acid (HCL) solution
e) 1.0L of 1M CaCL2 solution
f)
PROCEDURES:
1. Obtain a sample as in Section 4.4.
2. Prepare exactly 100mL of sample in a conical flask.
3. Add 150mL of CaCL2 solution into the sample, and stir the mixture.
4. Filter out the CaCO3 formed (white powder).
5. Add 200mL of HCL 0.05M into the filtered CaCO3 powder and stir the
mixture.
6. Add 5-10 drops of phenolphthalein indicator into the mixture. If the
sample turns red immediately, no free CO2 is present. If the sample remains
colorless, titrate with the standard 0.10M NaOH solution.
7. Measure the volume of 0.10M NaOH required reaching the end point. The
end point occurs when a definite pink colour persists in the solution for
longer than 30 seconds.

Table 2A
SAMPLE TABLE FOR EXPERIMENT 1 & 2
Process
: Absorption
Air flow rate

L/min

CO2 flow rate

L/min

CO2 inlet composition

vol%

Liquid flow rate

L/min

Time
(min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75

Outlet gas

Outlet water

Vol % of CO2 in outlet gas

Vol. Of NaOH for


sample titration
(mL)

Vol% of CO2
in outlet water

APPENDICES B: EXAMPLE OF LAB COVER PAGE

FOUNDATION OF CHEMISTRY I LABORATORY REPORT

EXPERIMENT 1: WASTEWATER TREATMENT METHOD OF PALM OIL MILL EFFLUENT

TAN JULLY (GROUP NO. 4)

SCHOOL OF ENGINEERING
FACULTY OF ENGINEERING, ARCHITECTURE & BUILT ENVIRONMENT

11 DECEMBER 2008

APPENDICES C: REFERENCE
Reference Style

The details of the references cited in the text, published or unpublished should be
located in the List of References. The list should be placed at the end of the thesis, a listing of
sources actually cited, compiled either alphabetically (Harvard System) or numerically
(Number System). The style selected must be used consistently throughout the thesis.

Author and Year System


This system is also known as Harvard System.

Citing in the Text

The references cited in the text should be indicated using the name of the author and
the date of publication. Examples are as follow:

(a) If the name of an author is written as part of a sentence, the year published should be
written in parentheses.

Works by Yao (1993) have shown that in order to maintain the behavioural link between the
offsprings and their parents, the use of crossover operator should be avoided.

(b) If the name of an author is not written as part of a sentence, both the name and year
published should be written in parentheses.
ANN offers useful properties and capabilities such as non-linearity, input and output
mapping, adaptability and fault tolerance among others (Haykin, 1999).

(c) If there are two authors for a cited reference, both names should be written.

In designing the model for non-linear system, the parsimonious principle (Soderstrom and
Stoica, 1989) is critical because a nonlinear model involves an excessive number of
parameters. Syu and Chang (1999) successfully used neural networks to adaptively control
Penicillin acylase fermentation.

(d) If there are more than three authors for a cited reference, use et al. after the name of the
first author.

The algorithm can be calculated by applying Gram-Schmidt procedures as described by


Korenberg et al. (1988).

(e) If more than one reference materials by the same author in a same year are cited, use
small letter alphabets (a, b, c, and so on) to distinguish them.

Some of the basic principles widely used by many researchers are Lagrange-Euler (LE)
equations (Uicker, 1965; Bejczy and Paul, 1981), Newton-Euler (NE) equations (Luh et al.,
1980a) and dAlembert (GD) equations (Lee et al., 1983).

Luh et al. (1980b) presented an example of an acceleration control of robot


arm/manipulator.

(f) Cross referencing in not allowed in a thesis. Only primary sources should be used.
Writing Style for Authors Names in the List of References

Generally, authors names are listed using surname followed by their initials. The followings
are examples of writing style according to the name of the author:

(i) Single and multiple authors

Example (single author) :

Veres, S. M. (1990). Structure Selection of Stochastic Dynamic Systems. New York:


Gordon and Breach Science Publishers.

Example (two or more authors):


Soderstrom, T., and Stoica, P. (1989). System Identification. United Kingdom:
Prentice Hall International Ltd.

Luh, J. Y. S., Walker, M. W., and Paul, R. P. (1980b). Resolved-Acceleration Control of


Mechanical Manipulators. IEEE Trans. Automatic Control. 25(3): 468-474.

(ii) Editor

Example:

Martin, A. M. (Ed.) (1991). Peat as an Agent in Biological Degradation of Waste. London:


Elsevier.

Lees, R. H. and Thomas T. R. (Eds.) (1974). Chemical Nomenclature Usage. Chichester:


Ellis Horwood.

(iii) Corporate author/editor

Example:

Engineers Joint Council (1969). Thesaurus of Engineering and Scientific Terms. New York:
Engineers Joint Council.

Writing Style for Various Types of Publication Materials in the List of


References

Frequently, different types of publication materials are cited in a thesis. The style of
writing details on cited publication should be as follows:

(i) Book

Author (Year). Title. (Edition). Placed published: Publisher.

Example:
Theusen, G. J. and Fabrycky, W. J. (1984). Engineering Economy. (6th ed.) Englewood
Cliffs, N. J.: Prentice Hall.

(ii) Article in a book

Author of the article (Year). Title of the article. In author or editor of the book. Title of the
book. (page). Place published: Publisher.
Example:
Hussein, S. B., Jamaluddin, H., Mailah, M. and Zalzala, A. M. S. (2000). An Evolutionary
Neural Network Controller for Intelligent Active Force Control. In Parmee, I. C. (Ed.)
Evolutionary Design and Manufacturing (pp. 351 362). London: Springer-Verlag.

(iii) Journal articles

Printed format
Author (Year). Title of the article. Title of the Journal. Volume (Issue no.), page.
Example:
Billings. S. A. (1980). Identification of Nonlinear Systems: A survey. Proc. IEE, Part D.
127(6), 272-284.

Electronic format
Author (Year). Title of the article. Title of the Journal. Volume (Issue no.), page. Publisher.

Example:
Borman, W. C. (1993). Role of Early Supervisory Experience in Supervisor Performance.
Journal of Applied Psychology, 78, 443 449. American Psychology Association.

(iv) Conference articles

Author (Year). Title of the article. Name of the conference. Date of the conference. Place,
page.

Example:
Sheta, A. F. and De Jong, K. (1996). Parameter Estimation of Nonlinear Systems in Noisy
Environments Using Genetic Algorithms. Proceedings of the 1996 IEEE International
Symposium on Intelligent Control. 15-18 September. Dearborn, Michigan: IEEE, 360 - 365.

(v) Thesis

Author (Year). Title of the thesis. Thesis award. Place published.

Example:
Adnan bin Hassan (2002). On-line Recognition of Developing Control Chart Patterns. Ph.D.
Thesis. Universiti Teknologi Malaysia, Skudai.

(vi) Legislations

Name of the country (year). Title of the legislation. Legislation number.

Example:
Malaysia (1983). Perintah Monumen Lama dan Tapak Tanah Bersejarah. P.U.(A)41 1983.

(vii) Standards

Name of the institution (Year). Standard number. Place published: Publisher.

Example:
British Standards Institution (1990). B.S. 764. London: British Standards Institution.

(viii) Patent

Print format

Author (Year). Patent number. Place published: Official source.

Example:
Smith, I. M. (1988). U.S. Patent No. 123, 445. Washington DC: U.S. Patent and Trademark
Office.
Electronic format
Author (Year). Patent number. Retrieved on date, year, from URL address of the patent
database.

Example:
Ulrich, K. (2001). European Patent No. EP1162184. Retrieved on March 7, 2002, from
fttp://ep.espacenet.com/

(ix) Brochure

Name of organization (Year). Title [Brochure]. Place published: Publisher.

Example:
Research and Training Center (1993). Guidelines for Reporting and Writing About People
with Disabilities. [Brochure]. Lawrance, KS: Macmillan.

(x) Measured drawings

Author (Year). Title. [Measured drawing]. Name of organization: Place published.

Example:
Salim Man (1989). Pengisi Sekam ke Dalam Kontena Penyimpan: Pandangan Isometrik.
[Lukisan Teknik]. Universiti Teknologi Malaysia: Skudai.

(xi) Unpublished materials

Author (Year). Title. Unpublished note, Name of organization.

(xii) Newspaper article

Print format
No author
Title of article. (Year, date). Name of newspaper, page.

Example:
Gearing up to meet new challenges. (2000, February 22). The Star. p. 2.

With author
Author. (Year, date). Title of article. Name of newspaper, page.

Example:
Izatun Shari (2000, April 18). K-economy: draft out in October. New Straits Times. p. 2-4.

Electronic format
Author. (Year, date). Title of article. Name of newspaper, Retrieved date, year, from URL
address of the newspaper.

Example:
Rosmawati Mion (2006, June 17). Sindiket judi haram tumpas. Utusan Malaysia. Retrieved
June 19, 2006, from http://www.utusan.com.my

(xii) Magazine

Author. (Year). Title of article. Name of magazine, Volume/Issue no., page

Example:

Smith, B. L. (1994). Biofeedback. Science, 62, 673 675.

(xiii) CD-ROM

Author. (Year). Title of article. [CD-ROM]. Title of Journal,, Volume, page. Publisher.

Example:
Ivry, R. B. (1995). Perception and production of temporal intervals across a range of
durations. [CD-ROM]. Journal of Experimental Psychology, 21, 3-18. American
Psychological Association.