mass transfer lab manual 2016

7/24/2019 Mass Transfer Lab Manual 2016

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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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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


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


29/44

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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35/44


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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.

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