[SEGi University]

Bachelor Degree of Chemical Engineering

Chemical Engineering Laboratory IV
Hand Book

SEGi University
TABLE OF CONTENTS

1.0 Introduction (Flow Chart)

2.0 Safety
3.0 Laboratory Report
3.1 Writing
3.2 Template
4.0 Marking Scheme
4.1 Rubric for Lab Report
4.2 Rubric for Lab Practical
5.0 Penalties
5.1 Late in Class
5.2 Report Late Submission
6.0 List of Experiments
7.0 Lab manuals
 The objective of this manual is to introduce the basic principles and methods of
experimental engineering to the lecturer who is allocated to teach Chemical Engineering
Laboratory II in Chemicall Engineering Department.

This section consists of three flow charts that indicate the procedures to conduct lab
investigations.
Figure 1.1 shows sequence of procedures to be taken if a lecturer is assigned to teach lab
investigations subject.

Figure 1.2 indicates the activities which are needed to be performed in the first lesson of
Lab Investigations. As an introductory class, regulation of lab, list of experiment/syllabus,
report writing skill and template, marking scheme and penalty has to be clearly explained to
students.

Figure 1.3 explains the procedures of activities during experiment. Lecturer has to ensure
the students are overall well prepared and have satisfactory knowledge of the expected task in the
laboratory.
 If allocated to teach lab investigations

Get the list of experiments

Study the relevant lab manual

Contact person-in-charge for relevant discipline

(refer to FC 2)

Test run the lab before conduct it

Figure 1.1 Actions Taken if Allocated to Teach Lab Investigations

 Introduction (refer to Section 1)

Distribute list of experiment (refer to Section 6)

Distribute lab manual (refer to Section 7)

Show the lab report format (refer to Section 3)

Review lab report writing skill (refer to Section 3)

Explain marking scheme (refer to Section 4)

Tell the penalty for late in class and report late submission (refer to Section 5)

Ask students to buy lab coat (refer to Mr. Teoh)

Inform students in advance about the next lab

Figure 1.2 Activities in First Lesson of Lab Investigations

 Take students' attandance

Check students' dress code

Brief experimental method and safety procedures

Supervise students to conduct the experiment

(observe students' performance and evaluate with Rubric 2)

Discuss on the obtained results

Inform students in advance about the next lab

Figure 1.3 Activities during Conducting Experiment

 Safety is of the most importance in the laboratory. Because students will be working with
hydraulic machinery powerful enough to pull apart thick steel rod, at temperatures high enough to
melt metallic alloys, at voltages large enough to induce dielectric breakdown in insulators, and
frequently with hazardous chemicals dangerous enough to suffocate and/or burn human body
instantly, safety is essential. If students have any doubt and questions about safety, stop
immediately what have been doing and consult Teaching Assistants/Coordinators. In order to
avoid or at least minimize the risk of an accident the followings are requested. Students not
complying with these simple rules will be asked to leave the session.

(1) Know where the fire extinguisher is located in the laboratory.

(2) Must wear shoes.
(3) Do not wear loose clothing.
(4) Long hair should be tied behind the head.
(5) Safety goggles must be worn around testing equipment, rotating machinery, and
chemicals.
(6) Do not consume food or drink, in the laboratory.
(7) All experiment must be performed within the allocated time. Students are not allowed
to work in the laboratory without proper supervision
3.1 Writing Skill

Each student is required to prepare a written report at the conclusion of every experiment. The
reports must always be brief, but yet provide sufficient information to convey to the reader that
you understood the principles and techniques involved. The reports for this course should never
exceed 5-10 equivalent typed pages. Note that the largest percent of your final grade will be
determined by the report of each student's laboratory experiment.

A plagiarized report (whether in part or in full) including copying from other sources, from
reports prepared by other groups, including another student in particular, will not be allowed and
will result in a zero grade. All reports MUST be handed in to the Teaching Assistant in charge by
the days of the week following the experiments. These reports should conform to acceptable
standards of report writing. The type of information in your reports will vary from one experiment
to another, but your reporting style should always state the purpose, background, technique, and
results as clearly as possible. Your reports should always contain a cover page, short abstract, brief
introduction, main body, and summary/conclusions.
A typical format for laboratory reports is given below:
1. The Title Page
The experimental title needs to contain the name of the experiment, the names of lab
partners/group, and the date of submission, name of marker, name of college and the institution.
Titles should be straightforward, informative, and less than ten words.

2. The Abstract/ Summary

A tightly written abstract summarizes four essential aspects of the report: the purpose of the
experiment (sometimes expressed as the purpose of the report), key findings, significance and
major conclusions. The abstract often also includes a brief reference to theory or methodology.
The information should clearly enable readers to decide whether they need to read your whole
report. The abstract should be one paragraph of 100-200 words.

3. The Introduction/ Theoretical Background

This is to place the work in the perspective of prior work including key literature survey. It states
the objective of the experiment and provides the reader with background to the experiment. State
the topic of your report clearly and concisely, in one or two sentences. A good introduction also
provides whatever background theory, previous research, or formulas the reader needs to know.
Usually, an instructor does not want you to repeat the lab manual, but to show your own
comprehension of the problem.

4. Experimental Methods and Materials (or Equipment)

An account of how experiment was carried out. It can usually be a simple list, but make sure it is
accurate and complete. In some cases, you can simply direct the reader to a lab manual or standard
procedure. Always use the third person and the past tense to describe what was done. Do not copy
from the handbook, which, in any case, is not an account of the method, but a set of instructions.
Do not waste time drawing elaborate sketches of the equipment unless it is vital to what you are
trying to describe. A simple line drawing is sufficient.

5. Results and Analysis

This should include a complete listing of your experimental readings, any data manipulation,
required graphs, etc. Calculations, tables and figures usually dominate results; however, you still
need to state all significant results explicitly in verbal form. Graphics need to be clear, easily read,
and well labeled. An important strategy for making your results effective is to draw the reader's
attention to them with a sentence or two, so the reader has a focus when reading the graph. All
columns and axes should be labeled with the variable name and its units.

6. Discussion
This is the most important and crucial part of your report, because here, you show that you
understand the experiment beyond the simple level of completing it. Explain. Analyze. Interpret.
Some people like to think of this as the "subjective" part of the report. By that, they mean this is
what is not readily observable. You should not confined yourself just to these points, but consider
other aspects of the experiment.

7. Conclusions
The conclusions represent a summary of the important findings in the experiment. It can be very
short in most undergraduate laboratories. There can be more detail than in the summary at the
front of the report, but any conclusions should be clearly and concisely stated. Simply state what
you know now for sure, as a result of the lab. Do not introduce any new material here; any
conclusions must refer to material that already discussed in the earlier report.

8. References
Any reference used must be mentioned in the main report and as part of a complete list at the end
of the reports. The reference list should give the author, the title of the publication and the date of
publication.

3.2 Report Template

This section consists of report writing template. A softcopy of report template should be provided
to students.

Font format for the lab report:

Font type: Times New Roman

Font size: 12

Font colour: Black

Spacing: Line spacing 1.5, before and after 0 pt

[SEGi University]

[ChemicalEngineeringLaboratory IV]

SEGi University

EXPERIMENT TITLE
Candidate’s Name:
Student ID:
Group Member’s Name:
1. Abstract
2. Introduction/ Theoretical Background
2.1. ABCDEF
Lorem ipsum dolor sit amet, consectetur adipiscing elit. In vel diam erat, vel
condimentum dolor. Curabitur et eros tellus. Aliquam varius, eros venenatis porta
vestibulum, lacus leo tempor odio, at congue tellus magna quis lacus. Vivamus
Suspendisse imperdiet eros eu sapien aliquam sed aliquam ipsum condimentum. Nam
suscipit euismod libero ac lobortis.

2.2. ABCDEFG
Lorem ipsum dolor sit amet, consectetur adipiscing elit. In vel diam erat, vel
condimentum dolor. Curabitur et eros tellus. Aliquam varius, eros venenatis porta
vestibulum, lacus leo tempor odio, at congue tellus magna quis lacus. Vivamus
Suspendisse imperdiet eros eu sapien aliquam sed aliquam ipsum condimentum. Nam
suscipit euismod libero ac lobortis.
2.3. ……..
3. Experimental Method
3.1. Equipments
 3.2. Cautions
3.3. Method/steps
4. Results and Analysis
4.1. Pressure versus flow rate graph
4.2. Flow rates versus coefficient
4.3. ….
5. Discussion
5.1. …….
5.2. …..
6. Conclusion

7. References ( Following Havard Referencing)

(a) 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.
(b) 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.
(c) Journal articles
Author (Year). Title of the article. Title of the Journal. Volume: page
Example:
Borman, W. C. (1993). Role of Early Supervisory Experience in Supervisor Performance.
Journal of Applied Psychology. 78: 443 – 449.
(d) Conference articles
Author (Year). Title of the article. Name 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. Dearborn, Michigan. 360 - 365.
Harvard Reference List Citations for Websites

When citing a website, use the following structure:

● Last name, First initial (Year published). Page title. [online] Website name. Available at:
URL [Accessed Day Month. Year].

When no author is listed, use the following structure:

● Website name. (Year published). Page title. [online] Available at: URL [Accessed Day
Mo. Year].

Example:

● Messer, L. (2015). 'Fancy Nancy' Optioned by Disney Junior. [online] ABC News.
Available at: http://abcnews.go.com/Entertainment/fancy-nancy-optioned-disney-junior-
2017/story?id=29942496#.VRWbWJwmbs0.twitter [Accessed 31 Mar. 2015].

● Mms.com. (2015). M&M'S Official Website. [online] Available at: http://www.mms.com/

[Accessed 20 Apr. 2015].
 This section prepares marking schemes to evaluate student’s lab report and lab practical
performance. Student’s lab report is evaluated by using Rubric 1; lab practical performance is
evaluated by using Rubric 2.

Score breakdown:

Score Breakdown
Categories: Score ratio Sub categories Details
(100/100)
Guided Laboratory Practical 80%
50% Lab Work Performance
Experiment Report 20%
Practical/
Open Ended Lab 50% Lab Work/Presentation 100%
Report
4.1. Rubrics for Lab Report (Overall Score Ratio: 80/100)

Mark
Evaluated Weight
No
Items Factor
0 2 4 6 8

Does not Follows Follows Follows Fol

General
1 0.05 follow guidelines guidelines guidelines gui
Layout
guidelines. poorly. satisfactorily well ext

Does not Topic is Topic is Topic is To

Not
2 Title 0.05 follow indicated indicated indicated ind
indicated.
guidelines. poorly. satisfactorily well. ext

No
Abstract/ Summary is Poor Satisfactorily Good Ve
3 0.1 summary is
Summary incomplete. summary. summary. summary. sum
provided.

Purpose and Purpose and Purpose

Pur
scope are scope are and scope
Neither sco
defined defined are defined
purpose Purpose and def
Introduction/ poorly. satisfactorily well.
4 0.2 nor scopes scope are ext
Background Background . Provide Provide
are incomplete. Th
information background adequate
provided. bac
provided is without background
and
irrelevant. context. and context.

Wr
Not written Written in
No Not written Written in ten
in past past tense.
Experimenta procedure in past tense. past tense. Ex
5 0.1 tense. Missing
l Procedure has been Steps are Missing key det
Missing key minor
provided. illogical steps. com
steps. steps.
.
 Disorganize Slightly Data is
Data is
d organized organized Ex
Results: organized
No Results presentation presentation well. pre
Figures, well.
6 0.2 have been of data. . Missing Missing sup
graphs, Missing
provided. Missing essential some minor dat
tables, etc some major
essential support support for
support data.
support data. data. data.

Paragraphs
Information Paragraphs Par
are relevant
lacks clear have rele
and support
direction. direction but sup
No purpose.
No relevant Information are too broad pur
informatio Ideas are
7 Discussion 0.2 information does not for the scope are
n is not fully
is provided relate to of the paper. dev
provided. developed.
topic. No Some Ex
Good
Sources of sources of sou
sources of
error error. err
error.

Conclusions Conclusion
Conclusions Co
No are logical. s are
Conclusions are illogical. are
conclusion Topic is logical.
8 Conclusion 0.05 are Topic is To
s are summed up Topic is
incomplete. summed up sum
drawn. satisfactorily summed up
poorly. ext
. well.

No References
References Re
references are provided
9 References 0.05 are pro
are in wrong
incomplete. pro
provided. format

Total
4.2. Rubrics for Lab Practical
(Overall Score Ratio: 20/100)

Evaluated Weight Mark

No
Items Factor 0 1 2 3

Late for 21 mins

Attendance
and
1 and 0.1 Late for 20 mins Late for 10 mins Punctual
above or absent
promptness
w/o reason.

Carry out
experiments Do bring lab
Do bring lab Do bring lab
by following Does not bring lab manual, have
manual but do not manual and use it
2 steps given in 0.2 manual during the it beforehand
use it during the during the
the experiment. use it fully du
experiment. experiment.
instruction the experime
sheets.

Comply with Dress proper

Not comply with Do not dress
safety Dressed properly lab and is ful
safety procedure properly for lab
procedures in for lab and follow complied wit
3 0.2 at all. Does not but often comply
workshops safety procedures safe procedur
dress properly for with the other
and most of the time. laboratories o
lab. safety procedures.
laboratories. workshop.

Often hindered
Ability to Extremely group progress Sometimes Always had a
4 work in 0.2 difficult to work but occasionally hindered group cooperative
group with. promoted progress. attitude.
progress.

All data collected Data collecting Use correct

are wrong due to method is not Data collecting method to co
Analysis of the completely method is correct data, recogni
5 0.3
data misunderstanding accurate and there and data are human error
of experimental are a number if mostly accurate. technical erro
method. error in the data. any) and corr
 them on the s
Data collecte
mostly correc

Total
26
5.1 Late in Class

Punctuality is evaluated in Rubric 2. However, the student who late more than 20 minutes is
considered absent for the lesson and cannot submit lab report.

5.2 Report Late Submission

Lab report is evaluated by using Rubric 1. However, the following penalties will be applied for
reports submitted after the deadline.

On time No penalty
1 day late Minus 25%
2 day late Minus 50%
3 day late Minus 75%
4+ day late Minus 100%

27
28
 6.0 List of Experiments

Year 2/Semester 1
Chemical
Area Title Objective Existing Equipment
Engineering Lab 4

Experiment 1: To determine the Continuous

(i)Separation Separation Continuous principle of separation Distillation Column
Distillation through distillation Unit. Model BP80-50
(ii) Particle column Portable
Technology Refractometer
Ethanol (95%)

Separation Experiment 2: To determine the Gas Absorption Unit,

Gas Absorption effectiveness of Air Compressor, CO2
Unit absorption through gas gas cylinder, Portable
absorption unit CO2 Gas Analyser

Separation Experiment 3: To determine the Liquid-liquid

Liquid-Liquid principle of separation Extraction Unit (With
Extraction Unit through liquid-liquid Extraction solvent
extraction unit Recovery)
Data Acquisition
Portable
Refractometer

Particle Experiment 4: Objective- Air Heater, Fluidized

Technology High The relationship between columns, DPT, air
Temperature pressure drop and the compressor
Fixed and flow rate through packed
bed.

29
 Fluidized Bed The pressure drop at
Unit minimum fluidized
velocity
To demonstrate the
drying process of the
solid particles.

30
31
FACULTY OF ENGINEERING & BUILT ENVIRONMENT

SUBJECT: ECE2334 CHEMICAL ENGINEERING LAB PRACTICE

EXPERIMENT 1: Distillation Column Unit

1.0 OBJECTIVE
Experiment 1(a):
● To determine the tray efficiency of a distillation system.

Experiment 1(b):
● To operate a batch distillation unit at constant reflux.
● To examine the change in top and bottom composition, and the height equivalent
theoretical plates (HETP) over time in a batch distillation.
● To carry out mass balance calculations on the distillation unit.

2.0 THEORY/INTRODUCTION
The principle for Bubble Cap tray distillation is the same as for normal distillation: when a liquid
mixture is heat so that it boils, the composition of the vapor above the liquid differs from the liquid
composition. If this vapor is then separated and condensed into a liquid, it becomes richer in the
lower boiling component(s) of the original mixture.

This is what happens in a Bubble Cap tray distillation column. A mixture is heated up, and routed
into the distillation column. On entering the column, the feed starts flowing down but part of it,
richer in lower boiling component(s), vaporizes and rises. However, as it rises, it cools and while
part of it continues up as vapor, some of it (enriched in the less volatile component) begins to
descend again.

32
 Figure 1. Simple continuous fractional distillation tower
Figure 1 shows a simple continuous fractional distillation tower for separating a feed stream into
two fractions, an overhead distillate product and a bottoms product. The “lightest” products (those
with the lowest boiling point or highest volatility) exit from the top of the columns and the
“heaviest” products (the bottoms, those with the highest boiling point) exit from the bottom of the
column. The overhead stream may be cooled and condensed using a water-cooled or air-cooled
condenser. The bottoms reboiler may be a stream-heated or hot oil-heated heat exchanger, or even
a gas or oil-fired furnace. In a continuous distillation, the system is kept in a steady state or
approximate steady state. Steady state means that quantities related to the process do not change
as time passes during operation. Such constant quantities include feed input rate, output stream
rates, heat and cooling rates, reflux ratio, and temperatures, pressures, and compositions at every
point (location). Unless the process is disturbed due to changes in feed, heating, ambient
temperature, or condensing, steady state is normally maintained. This is also the main attraction
of Bubble Cap tray distillation, apart from the minimum amount of (easily instrumentable)
surveillance; if the feed rate and feed composition are kept constant, product rate and quality are
also constant. Even when a variation in conditions occurs, modern process control methods are
commonly able to gradually return the sieve tray process to another steady state again.

Since a Bubble Cap tray distillation unit is fed constantly with a feed mixture and not filled all at
once like a batch distillation, a Bubble Cap tray distillation unit does not need a sizable distillation
port, vessel, or reservoir for a batch fill. Instead, the mixture can be fed directly into the column,

33
where the actual separation occurs. The height of the feed point along the column can vary on the
situation and is designed so as to provide optimal results.

Design and operation of a distillation column depends on the feed and desire product. Given a
simple, binary component feed, analytical methods such as the McCabe-Thiele method or the
Fenske equation can be used to assit in the design. For a multicomponent feed, computerized
simulation models are used both for design and subsequently in operation of the column as well.
Modeling is also used to optimize already erected columns for the distillation for mixtures other
than those the distillation equipment was originally designed for.

The column can be fed in different ways. If the feed is from a source at a pressure higher than the
distillation column pressure, it is simply fed into the column. Otherwise, the feed is pumped or
compressed into the column. The feed may be a superheated vapor, a saturated vapor, a partially
vaporized liquid-vapor mixture, a saturated liquid (i.e, liquid at its boiling point at the column’s
pressure), or a sub-cooled liquid. If the feed is a liquid at much higher pressure than the column
pressure and flows through a pressure let-down valve just ahead of the column, it will immediately
expand and undergo a partial flash vaporization resulting in a liquid-vapor mixture as it enters the
distillation column.
Although small size units, mostly made of glass, can be used in laboratories, industrial units are
large, vertical, steel cylinders known as “distillation towers” or “distillation column”. To improve
the separation, the tower is normally provided inside with horizontal plates or trays. To provide
the heat required for the vaporization involved in distillation and also to compensate for heat loss,
heat is most often added to the bottom of the column by reboiler, and the purity of the top product
can be improve by recycling some of the externally condensed top product liquid as reflux.
Depending on their purpose, distillation columns may have liquid outlets at intervals up the length
of the column
Large-scale industrial fractionation towers use reflux to achieve more efficient separation of
products. Reflux refers to the portion of the condensed overhead liquid product from a distillation
tower that is returned to the upper part of the tower as shown in figure 3 and figure 4. Inside the
tower, the downflowing reflux liquid provides cooling and partial condensation of the upflowing
vapors, thereby increasing the efficiency of the tower. The more reflux that is provided, the better
is the tower’s separation of the lower boiling from the higher boiling components of the feed. A
balance of heating with a reboiler at the bottom of a column and cooling by condensed reflux at
the top of the column maintains a temperature gradient (or gradual temperature difference) along
the height of the column to provide good conditions for fractionating the feed mixture.

34
 Changing the reflux (in combination with changes in feed and product withdrawal) can also be
used to improve the separation properties of a sieve tray distillation column while in operation (
in contrast to adding plates or trays, or changing the packing, which would, at a minimum, require
quite significant downtime).
Total reflux condition is often used to determine feasibility of a distillation system by obtaining
the tray or plate efficiency.
There are three types of tray or plate efficiency used:
i. Overall Tray Efficiency, Eo,
number of ideal trays
Eo 
number of actual trays
ii. Murphree Tray Efficiency, EM
y n  y n 1
EM 
y * n  y n 1
iii. Local Tray Efficiency, EMP

y 'n  y 'n 1
EMP 
y *n  y 'n 1

35
 3.0 APPARATUS

Pressure Transmitter, PT,

P1
Condenser, W2

Phase Separator, B6
W2 Solenoid Valve, SV

Different Pressure
Transmitter, DPT

Column
Temperature
Sensor

Pressure Reducing
Valve,PRV

Reboiler, W1 Metering Pump, P1

36
 Figure 2: Continuous Distillation Column Unit

37
 Figure 3: Process flow diagram for continuous distillation column

38
4.0 OPERATING INSTRUCTIONS

4.1 Description and Assembly

The Continuous distillation column are made of borosilicate 3.3 glass with PTFE gaskets and
stainless steel. Please refer to the process flow diagram in Figure 1.

1. Reboiler (B1) – a 7 L horizontal reboiler equipped with two 1,000 W cartridge

heaters (W1a & W1b). The reboiler is supplied with liquid level switch LS-01,
a temperature probe TIC-201. The reboiler also comes with a charge port for
feeding. A drain valve is fitted at the bottom of the reboiler.
2. Bubble Cap Tray Column (K1a) – a DN 50 borosilicate column with 10 sieve
trays and equipped 10 temperature probes, which are TI-101 until TI-110. A
temperature probe TT-112 is available for distillate temperature measurement.
A differential pressure sensor is also provided to measure the pressure drop
across the Bubble Cap tray column. Column height: approx. 1 m.
3. Packed Column (K1b) – a DN 50 column packed with 8 mm Raschig Ring. A
temperature probe TT-112. is available for distillate temperature measurement.
A differential pressure transmitter is also provided to measure the pressure drop
across the packed column. Packing height: approx. 1 m.
4. Top Condenser (W2) – a high efficiency condenser with 0.5m2 exchange area
and cooling water connections.
5. Product Cooler (W3) – having 0.035 m2 exchange area and cooling water
connections.
6. Product Tank (B4&B5) – a 5 L graduated tank with venting connection and
valves.
7. Feed Tank (B2& B3) – a 5 L cylindrical tank with discharge and venting.
8. Metering Pump (P1) – having maximum 8 LPH flowrate

39
4.2 Instrumentation and Control

Table 1: Description of Tags in Figure 2& 3

Tag Description Units Range Accuracy

TT 101 to 0
Column temperature C 0.0-100.0 ± 0.1% FS
TT 110

0
TT 111 Feed temperature C 0.0-100.0 ± 0.1% FS

Top column 0
TT 112 C 0.0-100.0 ± 0.1% FS
temperature

Outlet of Reboiler 0
TT 113 C 0.0-100.0 ± 0.1% FS
temperature

0
TIC 201 Reboiler temperature C 0.0-100.0 ± 0.1% FS

FT Feed flowrate L/min 0.0-1.0 ± 0.5% FS

Timer based reflux

controller

Position 1 : Total
reflux
KS 01 s 0-9999 -
Position 2 : Total
distillate offtake

Position 3 : Timer
controlled reflux

DPT Differential pressure mmH2O 0-1000 ± 0.007% FS

W1a & 1b Heater power W 0-2000 ± 0.25% FS

LS 01 Reboiler level switch - - -

40
4.3 Safety and Maintenance

1. The unit must be operated under the supervision of an authorized staff who has
been properly trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
3. Feed stock which severely affect PTFE, PFA and borosilicate glass are not to
be used.
4. The system should not be subjected to shock, sudden impact, vibration,
additional load, or permanent external action of aggressive vapours.
5. Always check and rectify any leak.
6. Do not touch the hot components of the unit.
7. Be extremely careful when handling hazardous, flammable or polluting
materials.
8. Restore the system to operating conditions after any repair job.
9. Make sure the system is sufficiently ventilated when working at atmospheric
pressure.
10. Only a properly trained staff shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.
11. Before any servicing, shut down the whole operation and let the system to cool
down and be properly ventilated.
12. Do not use any coarse or abrasive cleaners on glass components.
13. Leaking couplings should be carefully retightened. Replace any gaskets or seals
if necessary.
14. Flush the system with clean water after operation.
15. For long period shut down, ensure the system is clean and free from water.
16. Do not operate the system in extreme high temperature.
17. Ensure reboiler pressure do not exceed 3.5 bar absolute.

41
5.0 OPERATING PROCEDURES

5.1 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.

5.2 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 3L 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 5L of mixture with same ratio as in the reboiler and fill 5L of
mixture in each feed tank (B2 and B3).
4. Make sure all the valve are properly close except V4, V5, V10, V11 and V12.
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.

42
 7. Open the main cooling water valve V11 and V12. Let the cooling water flow
into the condenser (W2) and product cooelr (W3).
8. Switch on the cartridge heaters W1a & W1b and set the heater power controller
to 1.0 kW.
9. Allow the liquid in the reboiler to boil. As the liquid boils, the liquid level in
the reboiler will start to drop.
10. 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.

11. Check that the condenser has sufficient cooling water flow to minimize
escape of vapor into the vent.
12. 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 ± 0.2°C fluctuation.
13. The unit now is ready for experiment

5.3 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 V11 and V12.
6. Turn off the main power on the control panel.

43
6.1 Experiment 1(a): Batch Distillation at Total Reflux

6.1 EXPERIMENTAL PROCEDURES

1. Perform the general start-up procedures (Section 5.2).
2. Set heater power control to 1.0 kW and set the reboiler temperature to
approximate 95oC.
3. Ensure the reflux control is 1 position. (total reflux)
4. As the top column temperature sensor TT 112 and bottom sensor TIC 201, reach
steady state, record the temperature.
5. Set the reflux control to position 2 (Total distillate offtake). Open valve V7 and
collect 10 ml sample distillate using conical flask. Close valve V7 and set the
reflux control to position 1. (Total reflux).
6. 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 V3 and collect 10 ml of sample bottom product
using conical flask.Close valve V3.
7. Measure the refractive index of the samples and record the value into data table.
8. 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.
9. For different liquid and vapor loading, adjust the heater power settings in W1a
and W1b according table below:
10. Wait for approximately 15 to 30 minutes and allow the distillation unit to
achieve new steady state. Repeat steps 3 to 8.

44
 Heater Power 1.00 kW 1.50 kW 2.00 kW
Distillate Temperature 0C
RI
Mole Fraction
Bottom Temperature 0C
product
RI
Mole Fraction
Tray Efficiency

6.2 ANALYSIS AND DISCUSSIONS

1. Use the sample table 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 McCabe-Thiele method.
3. Calculate the tray efficiency of the column with different heating power
4. Discuss the effect of heating power on tray efficiencies

45
Table 2. Result from Total Reflux of Batch Distillation

Heater Distillate Reboiler Product Tray Murphee

W1, W2 T(oC) Refract. Mole T(oC) Refract. Mole Efficiency, Eo Efficiency
power Index Fraction Index Fraction EM
(kW)
1.00
1.50
2.00

46
7.0 Experiment 1(b):Batch Distillation at Constant Reflux

7.1 EXPERIMENTAL PROCEDURES

1. Perform the general start-up procedures (Section 4.2).
2. Record initial volume and refractive index of the liquid mixture in the reboiler.
3. Set the heater power to 1.5kW and set point of TIC to 95oC.
4. Use Reflux Ratio at 3 by setting reflux timer to 10 second for set 1 and 30 second for
set 2
( Note: Set 1: Product liquid to tank B4 ; Set 2: Product liquid return to
column).
5. Set the reflux control to position 3. (Timer controlled reflux).
6. As the top column temperature sensor TT 112 and bottom sensor TIC 201, reach steady
state, record the temperature.
7. Open sampling valve V7 and collect 10ml of distillate sample using conical flask. Close
valve V7.
8. Adjust bottom overflow level. Open valve V3 and collect 10 ml of sample bottom
product using conical flask.Close valve V3.
9. 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.)
10. Record Refractive Index value every five minutes by repeating steps 5 to 9 until the
bottom sample RI values constant
11. Switch off heater power and allow the system to cool down to ambient temperature.
Optional Mass Balance Calculation:
12. Open drain valve V1 and collect all the liquid from the reboiler. Measure the volume
and refractive index of the liquid. Record all the values.
13. 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.)

47
 7.2 ANALYSIS AND DISCUSSIONS

1. 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.
2. Determine the theoretical number of plates for each sampling time in the
distillation column using the McCabe-Thiele method.
3. Calculate the height equivalent theoretical plates (HETP) by dividing the
effective column height with the number of theoretical plates.
4. Using the Rayleigh equation, calculate and plot the amount of ethanol left in
the evaporator against time.
Table 3. Result from Batch Distillation at Constant Reflux

Heater power:

Reflux ratio:

Time Distillate Bottom Product

(min)
T(oC) Refract. Mole T(oC) Refract. Mole
Index Fraction Index Fraction

48
8.1 Preparation of Refractive Index (RI) vs Composition Plot
8.2 Experimental Procedures
1. Obtain the following information:
Ethanol purity: vol%
Density of ethanol: g/ml
Density of water: g/ml

Use the information to calculate the ethanol purity as wt%.

Ethanol purity: wt%

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

Mass of ethanol Mass of water (g)Ethanol wt% Mole fraction ethanol

Refractive Index (RI)
mixture (g)

0 10.0

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

9.0 1.5

10.0 1.0

11.0 0.5

12.0 0

3. For each mixture, measure the RI for each mixture using refractometer.
4. Calculate ethanol wt% and the mole fraction ethanol.

49
 5. Plot the RI function of the ethanol mole fraction. This is the calibration curve
used for the experiments as well.

9.0 REFERENCES
a. McCabe, Smith & Harriott, “Unit Operations of Chemical Engineering”, McGraw Hill,
(Singapore), 2001.
b. Geankoplis C.J., “Transport Processes and Unit Operations”, Prentice Hall,
(Singapore), 1995.
c. Perry R.H., “Perry’s Chemical Engineers’ Handbook”, McGraw Hill, (USA), 1997.

.
FACULTY OF ENGINEERING & BUILT ENVIRONMENT

SUBJECT: ECE2334 CHEMICAL ENGINEERING LAB PRACTICE

EXPERIMENT 2: Gas Absorption

1.0 OBJECTIVE
Experiment 2(a) :

● To determine the pressure drop across a packed column as a function of air and water
flow rates through the column.
● To examine the relationship between the experimental pressure drop values and
correlated values for a packed column.
Experiment 2(b):

● To demonstrate the absorption of CO2 into water using a packed column.

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

2.0 THEORY/INTRODUCTION
Gas absorption is a unit operation in which soluble components of a gas mixture are dissolved in
a liquid phase. The inverse operation, called stripping or desorption, is employed when it is desired
to transfer volatile components from a liquid mixture into a gas phase. Both absorption and
desorption processes, common to distillation, make use of special equipment for bringing gas and
liquid phases into intimate contact.

This experiment is conducted to demonstrate the absorption of carbon dioxide into water in a
packed column. The gas and liquid normally flow countercurrently, and the packings serve to

50
provide the contacting and development of interfacial surface through which mass transfer takes
place.

Height of the tower is crucial in designing an absorption tower. The design of an absorption
column’s height can be based on any of the rate equations but the overall gas film coefficient, Kya
is often used. The choice of this overall gas film coefficient does not require any assumption about
the controlling resistances, and can be used accurately for both liquid and gas film controlling mass
transfer.

Gas outlet

ya
Liquid inlet

xa
Z
ZT
dZ

y x
Liquid outlet

xb
Gas inlet

yb

Figure 1: Diagram for packed absorption column

Referring to the packed column in Figure 1, the cross section area is S while the differential volume
in height dZ is SdZ. If the change in molar flow rate V is neglected, the amount absorbed in section
dZ is (–Vdy), which is equal to the absorption rate times the differential volume:

51
  V dy  K y a y  y * S dZ [1]

b
Kya S K y a SZ T dy
V  dZ  V

y y*
a [2]

The right hand side of equation [2] can either be integrated directly or determined numerically for
some cases.

By rearranging equation [2], the column height ZT can be defined as:

b
V /S dy
ZT 
Kya y y*
a [3]

The integral above represents the change in vapour concentration divided by the average driving
force and is called the number of transfer units (NTU), NOy. The part outside the integral in
equation [3] has the unit of length and is called the height of transfer unit (HTU), HOy. From the
transfer units, the height of a packed absorption column can be determined by calculating NOy from
the xy diagram and multiplying it by HOy obtained from literature or mass transfer correlations.

ZT  H Oy N Oy [4]

For straight and parallel operating and equilibrium lines, the number of transfer units is the same
as the number of ideal stages in a packed column.

yb  ya
N Oy 
y y* [5]

52
However, for straight but non-parallel operating and equilibrium lines, the number of transfer units
is the change in concentration divided by the logarithmic mean driving force.

yb  ya
NOy 
y L [6]

*
*
in which y L is the logarithmic mean of y b  y b and y a  y a . 

The overall height of a transfer unit can be defined as the height of a packed section required to
accomplish a change in concentration equal to the average driving force in that section. The values
of HOy must often be estimated from empirical correlations.

In general, there are four kinds of transfer units based on individual or overall driving forces:

V /S dy
Hy 
kya
Ny   y  yi
Gas film: [7a]

L/S dx
Hx 
kxa
Nx   x  xi
Liquid film: [7b]

V /S dy
H Oy 
Overall gas: Kya
N Oy  y y* [7c]

L/S dx
H Ox 
Overall liquid: Kxa
N Ox   x * x [7d]

The pressure drop occurs in a packed column due to fluid friction among the packings. In Figure
2 below, the pressure drop per unit packing depth is plotted on logarithmic coordinates against
the gas flow rate, Gy (mass per hour per unit empty column cross sectional area).

Increasing liquid flow rate

dry
53
g depth
 Figure 2 : Pressure drop in a packed column in logarithmic coordinates

When the packing is dry, the line is straight, thus giving a power relationship between pressure
drop and gas flow rate. However, if the packing is irrigated with a constant flow of liquid, the
relationship between pressure drop and gas flow rate initially follows a line parallel to that of dry
packing. This pressure drop is greater than that for the same gas flow rate in dry packing because
liquid in the column reduces the space available for gas flow. At higher gas flow rates, the line for
the irrigated packing gradually becomes steeper because the gas now impedes the down flowing
liquid. At a point in which liquid holdup starts to increase, the slope of the pressure drop changes.
This is called the loading point.

With a further increase in gas flow rate, the pressure drop rises rapidly until the lines become
almost vertical and the liquid becomes the continuous phase. This is called the flooding point, in
which liquid will accumulate at higher gas flows until the entire column is filled with liquid.

A widely used correlation for estimating pressure drops in packed column is shown in Figure 3,
with the following parameters:

L* w v
x-axis: V *w L [8]

54
  L 0.1
13.1(V * w ) 2 F p ( )
L
y-axis: v ( L  v )

Gy  
V *W 
A

V*w= gas mass flow rate per unit column cross-sectional area, kg/m2s

L*w= liquid mass flow rate per unit column cross-sectional area, kg/m2s

FP = packing factor

 L = liquid viscosity, Ns/m2

Water viscosity=0.001Ns/m2

 L ,  v = liquid and vapour density, kg/m3

A= Area

Density of water =996 kg/m3

Density of air = 1.175 kg/m3

Column Diameter: 80mm

Fp= 900 m-1

55
Figure 3: Generalized pressure drop correlation, adapted from a figure by the
Norton Co. with permission

56
 Figure 4: Process flow diagram for the gas absorption unit

3.0 APPARATUS

Please refer to the process flow diagram in Figure 4.

1. Sump Tank (B1)

Rectangular tanks with removable top cover and level sight tube

Capacity: 50-L

Material: stainless steel

Low level switch for protection of centrifugal pump from dry run

2. Sump Tank (B2)

Rectangular tank with removable top cover and level sight tube

Capacity: 50L

Material: stainless steel

3. Circulation Pump (P1)

Magnetic drive sealless centrifugal pump

Maximum Flowrate: 62 L/min @ 5.7m head

Output power: 65 W

Material: polypropylene (PP)

4. Absorption Column (K1)

Packed columns filled with Raschig rings

Diameter: 80 mm

57
 Effective packing height: 1.5 m

Material: Perspex and stainless steel

Packing: 10 mm glass Raschig rings

Column K1 comes with ports for pressure drop measurements

5. Portable Gas Analyzer (Q1-01)

Measuring range: 0-100 vol% CO2

Accuracy: ±2% CO2

4
9

3
1
2

7
6

Figure 5

No. Tag Description Range

58
 1 dPT-201 Column K1 pressure drop 0–500 mmH2O

2 FT-101 CO2 flow rate 2-20 L/min

3 FT-102 Air flow rate 1-12 CMPH

4 FT-103 Water flow rate 1-10 L/min

5 Sump tank B1 low level

LS-01 –
switch

6 P1 Circulating Pump 62 LPM

7 BI and B2 Sump tank 50L

8 K1 Packed Column -

4.0 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 flow meter 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

59
 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 except by-pass valve V4.
2. Check that all gas connections are properly fitted.
3. Open the valve at the air compressor. Set the supply pressure to between 2 to 3 bars by
turning the air filter regulator knob clockwise.
4. Open the valve at the CO2 gas supply. Set the supply pressure to between 0.2 MPa to 3
MPa by turning the gas regulator knob clockwise.

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 and B2 by opening valves V7 and V9.

4.4 Liquid Sampling Procedures

Samples can be taken from the liquid in the sump tank B2 for analysis. The sampling valve
is located at V8 for outlet liquid from absorption column K1.

The procedures for collecting a sample are as follows:

(i) Place a vial below the sampling valve.

(ii) Collect about 150 mL of sample using vial.
(iii)Use pipette to collect 100 ml of sample from the sample collected and analyze the
acidity of sample using method described in section 4.6.

60
 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 5–10 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.

5.0 EXPERIMENT 2(a) : Hydrodynamics of a Packed Column

5.1 PROCEDURES:

1. Perform the general start-up procedures as described in Section 4.2 except step 4.
2. Fill the sump tank B1 with 40-L of fresh water.
3. To run the experiment with dry column, open valve V2 to introduce air into the
column. Allow the air to flow through the column until all evidence of moisture in
the packing has disappeared.

61
4. Adjust valve V2 to fix the desired air flow rate at FI-101, starting at a low value.
5. Record the pressure drop across the packed column at dPT-201.
6. Repeat steps 4 to 5 above with increasing values of air flow rate from 1 m3/h to 12
m3/h.
7. Close valves V2.
8. To run the experiment with wet column, open valve V6. Partially open valve V4.
9. Switch on the circulation pump P1 and slowly open valve V3.
10. Observe water entering the top of the packed column K1, flowing down the column
and back into the sump tank B1. Adjust V5 to maintain the water level in the bottom
of column at ¾ height of the bottom vessel.
11. Adjust valve V3 to fix the desired water flow rate at FI-103, starting at a low value.
12. Open and adjust valve V2 to fix the desired air flow rate, starting at a low value.
13. Record the pressure drop across the packed column at dPT-201.
14. Repeat steps 11 to 12 above with increasing values of air flow rate from 1 m 3/h to
12 m3/h while maintaining the same water flow rate. Stop when flooding starts to
occur in the column.
15. Close valve V1. Repeat steps 10 to 13 above with increasing values of water flow
rate from 1 LPM to 3 LPM.
16. End the experiment by performing the general shut-down procedures as described
in Section 4.3 except step 4.

RECOMMENDATIONS:

Variables Range

Air flow rate 12 m3/h

Liquid flow rate 0-3.0 L/min

62
63
Table 1. Result from experiment 2(a)

Flow Rate Pressure Drop (mm H2O)

Air
(m3/h)
1 2 3 4 5 6 7 8 9 10
Water
(L/min)

64
Table 2. Theoretical result of flooding point

Gas Flowrate
V*w K4 FLV(1LPM) FLV(2LPM)
(m3/h)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

65
5.2 ANALYSIS & DISCUSSION:

1. Use the sample table given above for data collection.

2. For a dry column without flow of water, plot the column pressure drop against
the air flow rate in a log-log graph paper.
3. Establish a relationship between the pressure drop and the air flow rate in the
dry packed column.
4. For a wetted column, plot the column pressure drop against the air flow rate for
each water flow rates in a log-log graph paper.
5. Mark the loading point and flooding point on the wetted column plots.
6. Calculate the following parameters and obtain the pressure drop from the
generalized correlation chart in Figure 12.

Gx y
x-axis: G y x  y

G y2 FP  x0.1

y-axis: g c  x   y  y 

Compare between the experiment and correlated values.

66
6.0 EXPERIMENT 2(b): Absorption of Carbon Dioxide from Air into Water

6.1 PROCEDURES:

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

2. Fill the sump tank B1 with up to 40-L of fresh water. Fully open valve V4.
3. Open valve V6. 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, FI-101.
iii. Open and adjust valve V2 to set the flow rate of air, FI-102
5. Record the inlet CO2 composition (vol%) using portable CO2 gas analyzer.
Open valve V10 then put the delivery tube of the gas analyzer into the gas inlet
sampling port.
6. After measurement done, Close valve V10.
Optional: At the same time, record the initial CO2 concentration in the sump tank B1
as the feed composition value.
7. Introduce liquid into the absorption column K1 as follows:
i. Partially open valve V4 and slowly open valve V3.
ii. Observe liquid entering the top of the absorption column, flowing down
the column and back into the sump tank B2.
iii. Adjust valve V3 to fix the desired inlet liquid flow rate at FI-103
8. Record the outlet CO2 composition using portable CO2 gas analyzer, Q1-01.
Open valve V11 to then put the delivery tube of the gas analyzer into the gas
outlet sampling port.
Optional: At the same time, collecting liquid sample from the outlet liquid of the
absorption column K1. Analyze the collected sample to determine the
concentration of dissolved CO2 in water (Section 4.5).
9. Continue record the outlet CO2 composition at every 5-minutes interval until
there are no more changes in CO2 composition over time.
Optional: Continue collecting liquid sample at every 5-minutes interval until there are
no more changes in CO2 composition over time.
10. Throughout the experiment, monitor and maintain the air, CO2 and water flow
rate by adjusting appropriate valves.

67
11. Stop the experiment and perform the general shut-down procedures as
described in Section 4.3.
12. Repeat the experiment by changing the gas flow rate, gas inlet composition and
liquid flow rate.

RECOMMENDATIONS:

Variables Range

Air flow rate 3 m3/h

CO2 gas flow rate 4-8 L/min

Inlet gas composition 9-16 vol%

Liquid flow rate 4.0 L/min

68
 Table 3.0 Experimental Data for CO2 Absorption ( Conc. of CO2 =_____)
Time (min) CO2 Composition (vol%)
0 1 2 3 Average
5
10
15

69
 Table 3.1 Experimental Data for CO2 Absorption ( Conc. Of CO2=_____)
Time (min) CO2 Composition (vol%)
0 1 2 3 Average
5
10
15

70
 6.2 ANALYSIS & DISCUSSION:

1. Use the sample table in given above 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.

7.0 REFERENCES

1. Christie John Geankoplis, Transport Processes and Separation Process Principles, 4th edition,
New Jersey, Pearson Prentice Hall, 2003
2. Perry, R.H., and Green, D. Perry’s Chemical Engineers’ Handbook, 6th edition New York,
McGraw-Hill Book Company, 1984.

71
FACULTY OF ENGINEERING & BUILT ENVIRONMENT

SUBJECT: ECE2334 CHEMICAL ENGINEERING LAB PRACTICE

EXPERIMENT 3: Liquid-liquid Extraction: Extraction of Acetone from Water Using

Toluene

1.0 OBJECTIVES

● To operate a liquid / liquid extraction experiment using a packed column

● To determine the height equivalent theoretical plates (HETP) for the column
● To investigate the effect of the solvent to feed flow rate ratios on the HETP

2.0 INTRODUCTION/THEORY

The Liquid-Liquid Extraction Unit (Model: BP 61) has been designed to demonstrate the basic
principles of a liquid-liquid extraction process.

The normal mode of operation is that the light phase and heavy phase liquids are pumped
countercurrently into the packed extraction column. The heavy phase will enter the top of the
column and flow downwards while the light phase will enter the bottom of the column and flow
upwards due to density differences. Countercurrent flow among the packings in the column of the
two phases will cause the transfer of solute component from one phase (raffinate) to the other
(extract). The raffinate will emerge at the bottom while the extract will emerge at the top of the
extraction column. This liquid-liquid extraction process is carried out among the column packings
to give a higher degree of separation.

Sampling points are provided at key positions around the unit to allow collection of both light and
heavy phase liquids. In this way, effects of feed flow rates of both phases on the extraction
efficiency can be evaluated by means of sample analysis.

A process flow diagram of the unit is shown in Figure 1.

72
 Figure 1: Process Flow Diagram for the Liquid-Liquid Extraction Unit

When separation by distillation is ineffective or very difficult, liquid-liquid extraction is one of the
main alternatives to consider. Close boiling mixtures or substances that cannot withstand the
temperature of distillation, even under a vacuum, may often be separated from impurities by
extraction, which utilizes chemical differences instead of vapor pressure differences.

Separation by liquid-liquid extraction can be defined as the selective removal of one or more
components either from a homogeneous liquid mixture or from a solution, using a second liquid
or solvent, which is partially or wholly immiscible with the first.

The following terms are widely used to describe the different streams in a liquid-liquid extraction
system:

F : Feed

S : Solvent

R : Raffinate

E : Extract
EXTRACTION
PROCESS
solvent, S extract, E

solute

raffinate, R feed, F

Figure 2: Flow of Streams and Components in a Liquid-Liquid Extraction System

In an extraction process, a quantity of feed liquid, F is mixed with a quantity of solvent, S in an

agitated vessel, after which the layers are settled and separated. The extract may be lighter or

73
heavier than the raffinate, and so it may be shown coming from the top of the equipment in some
cases and from the bottom in others.

Since the feed is a two component system, by convention, the material to be extracted is commonly
referred to as the solute while the other component is generally referred to as the diluent.

The raffinate stream has the same components as the feed, though the proportions are different,
with the raffinate having a much lower solute concentration (leaner). An ideal unit with perfect
extraction will yield a raffinate which has only one component, that being pure diluent.

The liquid used to strip the solute from the feed is referred to as the solvent. However, solvent is
a general term and should not be confused with the feed solvent or diluent. The solvent after
becoming enriched in solute leaves the system as the extract.

It is also important to define the composition of the four streams and this may be done in several
ways:

a) Molar concentration = mol/dm3 (note numerically this is the same as kmol/m3)

b) Molal concentration = mol/kg
No. of moles A
c) Mole fraction, xA = Total no. of moles
No. of moles A
d) Mole ratio, xA/B = No. of moles B
Mass of A
e) Mass fraction, xA = Total mass
Mass of A
f) Mass ratio, xA/B = Mass of B
Note: Fractions and ratios are dimensionless and may also be expressed in percent (%).

The common basis used in most literatures are either mole or mass fraction.

Since liquid-liquid extraction involves a 3-component system, a graphical representation of the

liquid mixtures is usually employed. There are two graphical systems, namely:

a) Rectangular coordinates
b) Triangular coordinates

74
The rectangular coordinates are easier to plot, but the triangular coordinates offer a more
representative view of the component compositions. However, it is important to fix the basis for
the representation before doing any calculations.

This manual will assume a composition basis of mole fraction and plots all component
compositions in triangular coordinates.

75
 A

E
F

M
S R

C B

Figure 3: A Typical 3-Component System Representation on an Equilateral Triangular Diagram

The individual components of the chosen ternary system are usually represented by symbols as
follows:

A = Solute

B = Diluent

C = Solvent

The assignment of symbols are arbitrary. Confusion shall not arise as long as the apex for the
solute is at the top while the bottom apexes are for the solvent and diluent.

Referring to Figure 3, the curve on the triangular diagram is called the binodal or solubility curve
of the ternary system. The curve, which is essentially a combination of diluent-rich and solvent-
rich curves, separates the upper region of stable single phase mixture from the lower region of
unstable mixture, which tends to separate into two phases.

76
The compositions of extract, E and raffinate, R are connected by tie-lines having different slopes
(i.e. not parallel). The tie lines get shorter as they get away from the x-axis, and eventually they
converge at a point P (plait point). The point P is not normally the highest part of the curve.

The number of theoretical stages can be determined graphically by constructing operating lines
and tie-lines on the binodal/solubility curves, as outlined in Figure 4. Consequently, the effects of
different stirrer speeds and feed flow rates on the extraction efficiency can then be evaluated.

Figure 4: Operating Lines and Tie Lines Constructions for Determination of Extraction
Efficiency

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4.0 OPERATING PROCEDURES

4.1 General Start-Up Procedures

1. Prepare the following chemicals:

a) Feed (heavy phase): mixture of acetone-water solution at the desired composition
b) Solvent (light phase): pure toluene
2. Ensure that all valves are closed (screwed in).
3. Fill feed tank B2 with 5L to 20L of acetone-water solution and feed tank B1 with 10
to20 L of pure toluene solvent.
4. Turn on the main power at control panel.
5. Switch on feed pump P2. Allow the acetone-water solution (heavy phase) to enter the
column and fill to a level of about 5-15cm above the solvent inlet. Switch off pump P2.
6. Switch on solvent pump P1.
7. As the solvent (light phase) enters the column, carefully watch the interface level which
forms between the light and heavy phases. Maintain the interface level at 5-10 cm
above the solvent inlet by adjusting the height of the overflow tube.
8. Once the liquid starts to overflow at the top of the column, stops pump P1.
9. The unit is now ready for experiment.

4.2 General Shut-Down Procedures

1. Switch off pumps P1 and P2.

2. Open valves V4 to V8 to drain all liquid from the equipment.
3. Turn off the power for the control panel.

78
5.0 EXPERIMENT PROCEDURES

In this experiment, there are two feeds and two outlet flows from the column.
● Feed flows: Solvent: Toluene (light phase)
● Feed: Acetone-water mixture (heavy phase)
● Outlet flows: Extract: Toluene rich phase/ Raffinate: Water rich phase

1. Ensure that all equilibrium and calibration data are obtained.

2. Perform the general start-up procedures (Section 4.2).
3. Switch on pump P1 and P2 and control flowrate of toluene at 2L/h and flowrate of feed
solution at 5L/h using valve V1 and V2 respectively.
4. Allow both liquids to flow into the collection vessels B3 and B4 respectively. The
bottom product contains the water rich phase (raffinate) while the top product contains
the toluene rich phase (extract).
Note: Monitor the interface level. Maintain it at about 5–10 cm above the solvent inlet
by adjusting the height of the overflow tube, or switching off pump P1 temporarily.
5. Let the experiment run for a while to attain steady state.
6. Open valve V6 to collect a 10 mL sample of raffinate and open valve V4 to collect a
10 mL sample of extract.
Note: Take samples at suitable intervals and measure their refractive indices. When the
readings are consistent over time, steady state has been reached.
7. Record the refractive index of both samples at steady state and use the calibration
curves to determine the acetone (solute) composition in each phase.
8. Record all data in the sample table.
Repeat the experiment (steps 4 to 8) by using different ratio of solvent to feed flow
rates. Always fix the same feed composition throughout the whole experiment.
Note: Recommended flow rate for Pump 1, P1 and Pump 2, P2 are from 1 L/h to 8 L/h
for both pumps.

79
 Table 1. Data for Experiment

Feed Raffinate Extract

Solvent Solvent
flow Time HETP Separation
flow rate to feed
rate (min) Efficiency
ratio Solute Solute (mm)
(L/hr) Refract. Refract.
L/hr) Composition Composition
Index Index
(wt%) (wt%)

80
 6.0 Calibration procedures for liquid/liquid extraction experiment.
Determination of the bimodal/solubility curve.

Apparatus: Conical flask, measuring cylinder, titration apparatus, refractometer, dropper

Toluene Rich Phase

1. Prepare 6 homogenous mixtures of acetone and toluene according to the table below:

N Amount in Water Compositions wt% Refractive

o mixture (ml) added Index
Aceton Toluen (ml) Aceton Water Toluen
e e e e
1 16 4
2 14 6
3 12 8
4 10 10
5 8 12
6 6 14

2. Prepare apparatus for titration and fill buret with water.

3. Titrate the solution in the flask with water and continue titrating until cloudiness appears
and persists in the mixture. When this occurs, record the exact amount of water that has
been added.
4. Take some sample and measure the RI of the sample using refractometer. Take 3 series of
readings and record the average.
5. Repeat the steps (2-5) for all mixture and calculate the mass fraction of each component.
6. Plot the RI of each mixture vs acetone (solute) composition.

Water Rich Phase

1. Repeat steps as in toluene rich phase. In this procedure, toluene should be added. Prepare
6 homogenous mixture according to table:

N Amount in Toluene Compositions wt% Refractive

mixture
o (ml) added (ml) Index
Aceton Water Aceton Water Toluen
e e e
1 16 4
2 14 6
3 12 8
4 10 10

81
 5 8 12
6 6 14

ANALYSIS AND DISCUSSION:

1. Determine the required theoretical extraction stage from the liquid-liquid extraction
experiment results.
2. Calculate the height equivalent theoretical plates (HETP) of the extraction column for
different solvent to feed ratio.
Effective column height
HETP = No. of theoretical plates

3. From the available data, do a mass balance calculation around the extraction column
and obtain the extract and raffinate flow rates.
4. Calculate the separation efficiency for different solvent to feed ratios.
Amount of extracted solute
Efficiency = Amount of solute in feed

Extract flowrate  Extract composition

= Feed flowrate  Feed composition

5. Compare the HETP values or separation efficiency for different solvent to feed flowrate
ratios.

6.0 REFERENCES

1. McCabe, Smith & Harriott, “Unit Operations of Chemical Engineering”, McGraw

Hill, (Singapore), 2001.

2. Robert E. Treybal, “Mass Transfer Operations”, Third Edition, McGraw Hill Book
Co. (Singapore), 1980.

3. Robert E. Treybal, “Liquid Extraction”, Second Edition, McGraw Hill Series, 1963.

4. Institution of Chemical Engineers, “Standard Test Systems for Liquid Extraction”,

Second Edition, 1985.

82
FACULTY OF ENGINEERING & BUILT ENVIRONMENT SUBJECT:

ECE3441 CHEMICAL ENGINEERING LABORATORY IV

EXPERIMENT 4: High Temperature Fixed and Fluidized Bed

1.0 INTRODUCTION

The High Temperature Fixed and Fluidised Bed Unit has been designed for student
experiments on the characteristics of flow through a bed particles. The equipment design for
student’s to obtain visual understanding and quantitative results on the flow of fluid through
the fixed and fluidized bed of solid particles. The unit is capable of running air as the flow
medium. A high power air heater has been provided to host the inlet air up to 250oC.

The unit is also capable of demonstrating basic characteristic such as bed expansion, pressure
drop, aggregative and particulate fluidization, bubbling phenomenon, effect of fluidization on
hot air flow and drying of solid particles. Instruments are provided for the complete
measurement of flow rate, pressure drop and temperature.

A system at considerable importance in chemical and other process engineering fields is packed
column which is used for fixed bed catalytic reactor, adsorption of the solute, absorption, filter
bed, and so on. The packing materials in the bed may be spherical, cylindrical, irregular particles,
or various kind of commercial packing. The solid phase is stationary, as it is in a packed distillation
column; in some cases, the bed moves countercurrent to the gas stream, as it does in a pebble heater
or in some catalytic reactors.

Student should be able to experiment with this unit to determine:

The relationship between pressure drop and the flow rate through packed bed.

The pressure drop at minimum fluidised velocity.

83
To demonstrate the drying process of the solid particles.

84
Figure 1: Process flow diagram for the High Temperature Fixed and Fluidised Bed Unit (BP23-
P)

85
2.0 GENERAL DESCRIPTION

2.1 Unit Assembly

Figure 2: Unit Assembly High Temperature Fixed & Fluidized Bed Unit (BP23-P)

1. Heater 7. 2 way valve (V 1)

2. Electrical panel 8. Needle Valve (V 2)

3. Air Flowmeter (FT 1) 9. Temperature Sensor (TT 1)

86
 4. Air Flowmeter (FT 2) 10. Temperature Sensor (TT 2)

5. Needle Valve (V 3) 11. Column 1

6. Needle Valve (V 4) 12. Column 2

2.2 Safety Considerations

18. The unit must be operated under the supervision of an authorized staff that has
been properly trained to handle the unit.

19. All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.

20. Feed stock which severely affect borosilicate glass, PTFE, PP, PVC and
stainless steel are not to be used.

21. The unit should not be subjected to shock, sudden impact, vibration, additional
load, or permanent external action of aggressive vapours.

22. Always check and rectify any leak. Leaking couplings should be carefully
retightened. Replace any gaskets or seals if necessary.

23. Do not touch the hot components of the unit.

24. Make sure the surrounding is sufficiently ventilated when operating the unit.

25. Only properly trained staff shall be allowed to carry out any servicing.
Manufacturer's manual must always be observed.

26. Do not use any coarse or abrasive cleaners on glass components.

27. Completely drain and flush the unit if it is not to be used for a long period of
time. Do not allow any liquid to accumulate in the unit.
87
3.0 SUMMARY OF THEORY

3.1 Flow in Packed Bed

Certain geometric relations for particles are used in the derivations for flow in
packed beds. The void fraction or porosity in a packed bed is defined as

Some typical value of porosity for various porous materials is given in table
below:

Material Porosity Material Porosity

Berl saddles 0.68 – 0.83 Brick 0.12 - 0.34

Catalyst Granules 0.45 Cigarette filter 0.17 – 0.49

Coal 0.02 - 0.12 Concrete 0.02 – 0.07

Crushed rock, granular 0.44 – 0.45 Fiberglass 0.88 – 0.93

Leather 0.56 – 0.59 Limestone 0.02 – 0.20

Limestone (dolomite) 0.04 – 0.10 Raschig rings 0.56 – 0.65

Sand 0.31 – 0.50 Sandstone 0.08 – 0.40

Silica powder 0.013 – 0.051 Soil 0.43 – 0.54

Spherical packing,
0.36 – 0.43 Wire rings 0.68 – 0.76
shaken

88
Experimentally, the relationship between friction factor and Reynolds number
has been found to be reasonably modeled by:

89
 Range of Re fp Appellation

< 10 150/Re Blake - Kozeny

10 < Re < 104 150/Re + 1.75 Ergun

> 104 1.75 Burke - Plummer

For the packed beds Ergun defined the Reynolds number as:

For laminar flow, the Hagen – Poiseuille equation can be defined as:

The true ΔL is larger because of the tortuous path, and use of the hydraulic radius predicts too
large a superficial velocity, υ’. Experimental data show that the constant should be 150, which
gives the Blake-Kozeny equation for laminar flow, void frictions less than 0.5, effective particle
diameter Dp and NRe,p<10:

90
For highly turbulent the friction factor should approach a constant value. Also, it is assumed that
all packed beds should have the same relative roughness. Hence the final equation for turbulent
flow for NRe,p > 1000, which is called the Burke- Plummer equation becomes

Adding equation [4] for laminar flow and equation [5] for turbulent flow, Ergun proposed the
following general equation for low, intermediate, and high Reynolds numbers, which has been
tested experimentally:

3.1 Flow in fluidized bed

Two general types of fluidization, particulate fluidization and bubbling fluidization, can
occur. The packed bed expands when the pressure drop due to the upward flow of the fluid
through a granular unrestricted bed equal the weight of the packing. As the bed expands, it
retains its top horizontal surface with the fluid passing through the bed much as it did when
the bed was stationary.

3.1 Minimum velocity or porosity for particulate fluidization

When a fluid flows upward through a packed bed of particles at low velocities, the particles
remain stationary. As the fluid velocity is increased, the pressure drop increases according
to the Ergun equation [6]. Upon the further increases in velocity, conditions finally occur
where the force of the pressure drop times the cross-sectional area equals the gravitational
force on the mass particles. Then the particles begin to move and this is the onset of the
fluidization or minimum fluidization. The fluid velocity at which fluidization begins is the
minimum fluidization velocity, υ’mf in m/s based on the empty cross section of the tower
(superficial velocity).

91
The porosity of the bed when true fluidization occur is the minimum porosity for
fluidization, εmf. Some typical value of εmf for various materials given in table below:

3.2 Pressure drop and minimum fluidizing velocity

As the first approximation, the pressure drop at the start of the fluidization can be
determined as follows:

92
Figure 2: The Ergun equation for flow in packed beds, and the two related asymptotes, the
Blake-Kozeny equation and the Burke-Plummer equation.

93
4.1 GENERAL OPERATING PROCEDURES

4.2 General Start-Up Procedure (Column 1)

1. Pull out top of column cap carefully.

2. Fill the column with sample to the desired height (10 cm).

3. Close back the cap carefully. Be sure that the o-rings are well placed.

4. Place the column on the holder and secure the column using the screw
provided.

4.3 General Start-Up Procedure (Column 2)

1. Do not fill any popcorn seed inside the column 2 before temperature of the
column reach 150 oC.

2. Place the U-tube Holder on top of the column.

4.4 General procedure for setting the air manometer (FT1 & FT2)

1. Connect the PU tube from air compressor to the pneumatic fitting.

2. Adjust the air regulator to minimize before start experiment.

3. Valve V3 is to control flowrate for FT1 and Valve V4 is to control
flowrate FT2.

4.4 General Shut-Down Procedures

1. Switch off heater.

2. Let the process cold down to room temperature before off air compressor.
3. Remove all sample from both columns.( If semester break)
4. Turn off the power supply.

94
5.1 EXPERIMENT PROCEDURES

5.2 EXPERIMENT 1: Fluidization in packed column using air (Column 1)

OBJECTIVE:

▪ To determine the pressure drop at minimum fluidised velocity.

▪ To verify Ergun equation.

▪ Study the behavior of fluidized bed for various size of bed material.

PROCEDURES:

1. Fill the column K1 with alumina (mesh 60) to obtain bed height of 100mm.
Refer to section 4.1.

2. Connect air supply to the equipment.

3. Switch on air compressor and slowly adjust pressure regulator to 2bar.

Slowly adjust V3 to obtain air flow rate of 2 L/min at FT1.

4. Monitor if the fluidization has occurred or not. Record the flow rate and
pressure drop when fluidization begins to occur.

5. Continue the experiment with different air flow rate between 2 and 20 L/min
at 1 L/min increment.

6. Change the bed with another alumina of different mesh size. Refer to general
start-up procedure in section 4.1.

7. Repeat steps 1 to 6.

ANALYSIS & DISCUSSION:

1. Plot pressure drop, ΔP vs flow rate, Q.

2. Calculate the pressure drop, ΔP at minimum fluidized velocity and compare

with the experimental pressure drop, ΔP.

95
96
5.3 EXPERIMENT 2: High Temperature Fluidization in packed column using hot air
(Column 2)

OBJECTIVE:

▪ To study the effect of fluidization to the temperature of supplied hot air.

▪ To demonstrate the drying process of the solid particles.

PROCEDURES:

1. Connect air supply to the equipment. (Do not fill in popcorn seed inside the
column 2 before the temperature TT1 reach 160 oC)

2. Switch on air compressor and slowly adjust pressure regulator to 4bar. Fully
open valve V4 and slowly adjust V2 to obtain air flow rate of 45 L/min at FT
2.

3. Switch on the heater. Set the temperature controller to 250 oC. You will
notice that if FT 2 less than 40 LPM the heater cannot on. (Do not fill in
popcorn seed inside the column 2 before the temperature TT1 reach 160 oC)

4. Observed the Temperature sensor TT1. Start the stop watch, after 1.5 min
adjust the valve V2 to increase FT2 to 160LPM.

5. Once the TT1 reach 160 oC, pour in the popcorn seed inside the column and
observe the reaction. The popcorn seed will received the hot air and become
popcorn.

6. Continue the experiment with different air flow rate 160LPM to 200LPM.

6.1 REFERENCES

1. Geankoplis C.J., “Transport Processes and Separation Process Principles (includes

Unit Operation), 4th Edition.”, Prentice Hall, 2003.

2. Foust A.S., Wenzel L.A., Clump C.W., Mans L., Andersen L.B., “Principles of Unit
Operations, 2nd Edition.” John Wiley & Sons, 1980

97
 Given data:

Particle size, Dp = 250µm

Shape factor, Ø = 0.67 (shape edge particle)

Solid density, ρs = 3970 kg/m3

Fluid density (Air), ρf = 1.2 kg/m3

Dynamic viscosity (Air), µ = 1.82 x 10-5 Pa.s

Bed height = 0.1 m

Bed mass, mb = 346.65 g

Column 1 diameter, D = 4.58 cm

Tabulated Results:

Q Bed Experimenta Superficia Volum Packed Voidage Theoretica Percentag

(L/min Height l Pressure l Velocity, e Bed bed ,ε l pressure e of error
) ,L Drop (Pa) U (m/s) (m3) (kg/m3 drop (Pa) (%)
(mm) )
2
3
4

98
99