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MASS TRANSFER (EP203)
LABORATORY MANUAL
Lecturer/Instructor: _______________________________
Name :____________________________
Student ID :____________________________
Course :____________________________
FACULTY OF ENGINEERING, ARTCHITECTURE &
BUILT ENVIRONMENT
UCSI UNIVERSITY
2016
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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
2 Absorption Column
A Example of Front Page
B Example of Cover Page
C Reference Citing Method
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1 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.
2 LABORATORY PROCEDURE AND CONTROL
2.1Logbook
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.
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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) PLAGIARISM WILL NOT BE TOLERATED.
(c) 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.
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(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.
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Marks for each report shall be allocated as follows:
Items Unacceptable Satisfactory Good Excellent ScoreScore 1 2 3 4
ObjectiveandIntroduction
Objective areirrelevant or are notappropriate to theexperiment
Objective /introduction miss atleast one importantconsideration
Introduction andobjective are listed,importantexperimental detailsare covered, someminor details missing
Introduction andobjectives fullyaddressed.
Timeliness Report handed inmorethan two days late
Up to one day late Up to one hour late Report handed in time
Experimentalprocedures
Procedures do notaccurately list thesteps of the
experiment
Procedures are listed,but seem missingsome information,
some steps are notnumbered and/or arein incompletesentences.
Procedures are listed,importantexperimental details
are covered, someminor details missing
Procedures are listed inclear steps; each stepis numbered and in a
complete sentence.
Result: data,figures,graphs,tables, etc.
Figures, graphs,tables containerrors or are poorlyconstructed, havemissing titles,captions ornumbers, unitsmissing orincorrect, etc.
Most figures, graphs,tables OK, some stillmissing someimportant or requiredfeatures
All figures, graphs,tables are correctlydrawn, but some haveminor problems orcould still be improved
All figures, graphs,tables are correctlydrawn, are numberedand containtitles/captions.
Discussion/
Observation
Very incomplete or
incorrectinterpretation oftrends andcomparison of dataindicating a lack ofunderstanding ofresults
Some of the results
have been correctlyinterpreted anddiscussed; partial butincompleteunderstanding ofresults is still evident
Almost all of the
results have beencorrectly interpretedand discussed, onlyminor improvementsare needed
All important trends and
data comparisons havebeen interpretedcorrectly anddiscussed, goodunderstanding ofresults is conveyed
Conclusion Conclusionsmissing or missingthe important points
Conclusionsregarding majorpoints are drawn, butmany are misstated,indicating a lack ofunderstanding
All importantconclusions havebeen drawn, could bebetter stated
All importantconclusions have beenclearly made, studentshows goodunderstanding
Appearance
andformatting
Sections out of
order, report is nottyped/written usingthe appropriateformat
Sections in order,
formatting is roughbut readable
Lab report is mostly
typed/written usingthe appropriateformat, all sections inorder, formattinggenerally good butcould still be improved
Lab report is
typed/writtenin well-formatted, veryreadable.
Spelling,grammar,sentencestructure
Frequent grammarand/or spellingerrors, writing styleis rough andimmature
Occasionalgrammar/spellingerrors, generallyreadable with somerough spots in writingstyle
Less than 3grammar/spellingerrors, mature,readable style
All grammar/spellingcorrect and very well-written
Total Mark
Final ScorePercentage (%) = (Total Marks / 32)*10
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3 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 notwear 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 all ow students who do
not follow this rul e 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.
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PREPARATION OF A REFRACTIVE INDEX (RI) VS. COMPOSITION
PLOT
1. Prepare a set of mixtures containing ethanol and water within a specified range ofcomposition 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)
Mole
fraction
ethanol
Ethanol
Wt%
Mass of
ethanol (g)
Mass of
water
(g)
Refractive
Index (RI)
0 0
0 0
0 0
0 0
0 0
0 0
0 0
0 0
5 5
0 0
5 5
.0 0
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 rangeof mixtures. This will serve as the calibration curve for further experiments.
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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 reachapproximate 85oC.
3. Ensure the reflux control is 1 position. (total reflux)
4. As the top column temperature sensor TT 112, reach steady state, record thetemperature.
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 andcollect 10 ml sample distillate using conical flask. Close valve V9 and set thereflux control to position 1. ( Total reflux).
7. To collect bottom product sample, adjust the overflow U-tube to asuitable 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 intodata table.
9. Wait for approximately 15 to 30 minutes and allow the distillation unitto achieve new steady state.
10.Repeat steps 2 to 8 for different liquid and vapor loading, adjust theheater power settings according table below:
Heater Power
(kW)
1.00
1.50
2.00
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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 thetop and bottom compositions on the diagram and determine the
theoretical number of plates in the distillation unit using the McCabe-
Thiele method.
3. Calculate the height equivalent theoretical plates (HETP) by dividingthe effective column height with the number of theoretical plates.
4. Plot a graph of HETP vs. Heating Power and observe the relationship.
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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 abatch 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 thereboiler.
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 intodata 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 ambienttemperature.
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. Measurethe volume and refractive index of the distillate. Record all the values.
(Note: Remember to include all previous samples.)
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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 thepacked column.
3. Using the X-Y equilibrium diagram for ethanol-water system, mark thetop 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.
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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 CO2into water.
To determine the saturation composition of CO2in water.
To study the effect of gas flow rate, gas inlet composition and
liquid flow rate on the rate of CO2absorption.
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 intothe sump tank B1 via valve V4.
4. Introduce air and CO2mixtures into the absorption column K1 as
follows:
i. Determine the appropriate air and CO2gas 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 CO 2, FI-
101.
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.
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iii. Adjust valve V3 to fix the desired inlet liquid flow rate at FI-
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 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
CO2gas 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 CO2composition in the inlet water flow as a function of time.
3. Compare the CO2 composition plots for different gas flow rates, gasinlet compositions and liquid flow rates.
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EXPERIMENT 4: ABSORPTION OF CARBON DIOXIDE FROM
AIR INTO NaOH
OBJECTIVE:
To demonstrate the absorption of CO2into NaOH using a packed column To calculate the rate of absorption into NAOH To determine the saturation composition of CO2in NaOH To study the effect of gas flow rate, gas inlet composition and liquid flow
rate on the rate of CO2absorption.
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 CO2mixtures 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 thecollected 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.
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REMARK:
Procedure to clean the equipment after the usage of NaOH
I.
Drain all of the NaOH from the equipment by opening valves V3,
V4, V5, V6 and V7.II. After draining, close valve V7.
III. Fill the sump tank with 20L of 0.1M HCl.
IV. 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.
V. Drain all of the HCl by opening valves V3, V4, V5, V6 and V7.
VI. After draining, close valve V7.
VII. Fill the sump tank with 40L of fresh water.
VIII. 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.
IX. 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.
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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 ratio2) Determination of moisture content
In the report, students are required to include details of:
1) What happens in the drying process2) Factors affecting drying3) The role of air temperature4) 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.
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APPENDIX 1 (DISTILLATION COLUMN)
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Figure 1: Process flow diagram of continuous distillation column
V3
TT 102TT 101
TT 103
TT 104
TT 105
TT 106TT 107TT 108
TT 109TT 110
KS 01
112
201
301
B6Dosing tank
5-L
V11
W2Condenser
0.5m2
CW
B7Phase separator
V9
V1
B4Distillate
Product tank5-L
V7
Packed Column, K2DN50 x 1.0m
8mm Raschig ring
TIC
LS01
W1a, W1bImmersion
heater2 x 1kW
Reboiler
7-L
V2 B5BottomProduct tank
5-L
CW
P1Metering
pump
12 L/hr
V6
V4 V5
B2Feed tank
5-L
B3Feed tank
5-L
Vent /
Vacuum
TT
TT
111
V12
DPT
V-2
FTFI
101 101
FI
102
V8
V13
W3Product Cooler
V-1V10
B1Sieve Tray Column, K1DN50 x 1.0m
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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.
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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.
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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. The unit now is ready for experiment
4.3 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.
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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)
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Figure 2:X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm
0.0000
0.1000
0.2000
0.3000
0.4000
0.5000
0.6000
0.7000
0.8000
0.9000
1.0000
0.0000 0.1000 0.2000 0.3000 0.4000 0.5000 0.6000 0.7000 0.8000 0.9000 1.0000
Vapormolfraction
Liquid mol fraction
X-Y Equilibrium Diagram for Ethanol-Water System at 1 atm
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Table 2: HETP
Heater W1a
and W1b
power (1kW)
Distillate Bottom Product HETP
(mm)
Temp
(C)
Refr.
Index
(RI)
Mole
Fraction
Temp
(C)
Refr.
Index
(RI)
Mole
Fraction
1.00
1.50
2.00
1b) Table of result for experiment 2
Heater power :
Reflux ratio:
Time (min) Distillate Bottom product
Temp (C) Refr. index Mole fract. Temp (C) Refr. index Mole
fract.
0
10
20
30
40
50
60
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Figure 1: process flow diagram for the gas absorption unit
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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 CO2and air flowrates, and consequently the CO2composition 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.
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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 CO2compressor. 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 CO2gas 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.
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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 CO2in 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 CO2free 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 CO2is present. If the sample remains colorless, titrate
with the standard 0.05 M NaOH solution.
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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 CO2free 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 CaCL2solution
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 CaCL2solution into the sample, and stir the mixture.
4. Filter out the CaCO3formed (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 CO2is 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.
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Table 2A
SAMPLE TABLE FOR EXPERIMENT 1 & 2
Process : Absorption
Air flow rate : L/min
CO2flow rate : L/min
CO2inlet composition : vol%
Liquid flow rate : L/min
Time
(min)
Outlet gas Outlet water
Vol % of CO2in outlet gas Vol. Of NaOH for
sample titration
(mL)
Vol% of CO2
in outlet water
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
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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
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APPENDICES C: REFERENCE
Reference Style
The details of the references cited in the text, published or unpublished should belocated 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.
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(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.
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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.
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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. 351362). 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, 443449. American Psychology Association.
(iv) Conference articles
Author (Year). Title of the article. Name of the conference. Date of the conference. Place,
page.
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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
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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 TrademarkOffice.
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, fromfttp://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
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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. RetrievedJune 19, 2006, from http://www.utusan.com.my
(xii) Magazine
Author. (Year). Title of article.Name of magazine, Volume/Issue no., page
Example:
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Smith, B. L. (1994). Biofeedback. Science, 62, 673675.
(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.