UTM

Facr*lty of Chemical
ar*d, Energy
Engiuoeeri,ng
(FChE)
ULIIVERSITI IEKNOLOGI MALAYSIA

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 SEPARATION PROCESSES LABORATORY II
@TJHM
This laboratory manual is prepared by the Department of Chemical Engineering, Faculty
of Chemical and Energy Engineering for the Separation Processes Laboratory II (SKKK
3761). The purpose of this lab manual is to serve as guidelines to students, technical
staff and lab instructors to assist in performing and understanding the experiments in
Unit Operation.

Separation Processes Laboratory iI syllabus consists of a total of seven experiments;

sieving, Fluidized Beds, Vacuum Filtration, Tray Dryer, Spray Dryer, Evaporation,
Vapour-Liquid Equilibrium (VLE) and Climbing Film Evaporator, The topics covered in this
course are essentially particLlate solid separation processes, drying and evaporation
experiments. All the equipments are prepared to instill a clear understanding of the
concepts and principles learnt in Unit Operation I and Unit Operation II classes, The
theories lie in the subjects will be fully utilized in this Iaboratory,

In this coLlrse, chemical engineering students will be introduced to the application of the
semi-industry scale equipments as a preparation before entering the actual workplaces.
This course will give a'hands on'experience to the students on how to handle the
equipments and to interpret the data taken from the experiments, which provides
practical and informative exposure about operational mechanisms of separation
systems
that can be used in the chemical/bio-process industries.

This course is not only focused on conducting experimental works but it also emphasizes
on the development of team working skills. Maximal efficient use of teamwork skills is
required to complete each experiment on time and produce a quality work product. By
providing conducive laboratory environment, it enables promotion of positive interaction
and communication among students and lab personnel, which then can train them to be
a responsible and discipline person in any given situation, With these proactive attitudes,
the aim of creating professionalism at work can be achieved.

In order to be a successful process engineer, a student should have a clear vision and
make the best use of this subject to gain as much knowledge and experience as
possi b I e,
ry,Hth# SEPARATION PROCESSES LABORATORY II

I ),fN i f=i\i'i-.:

1. Preface
2. Table of Contents
3. introduction and Basics
4. Guidelines for preparing Lab Report
5. List of Experiments
6. Experiment 1: Sieving
7. Experiment 2; Fluidized Beds
B, Experiment 3: Vacuum Filtration
9. Experiment 4: Tray Drfer
10 Experiment 5: Spray Dryer
11. Experiment 6; Climbing Film Evaporation
72. Experiment 7: Vapour-Liquid Equilibrium (VLE)
ffitJxhf, SEPARATION PROCESSES LABORATORY II

Sttrd.erl't Lea rning Or{teorq,tes

At the completion of this course, students should be able to:

operate the equipment properly in order to obtain the significant data.

Calculate drying time for constant- rate and falling-rate period in drying process.
Study the characterization of solid particles and to calculate the average size and
size distribution of the particles using Tyler standard screen analysis in particle
technology.
Determine which equifment is suitable to separate any given type of particulate
solids.
Explain how the data is being generated and analyze data for each equipment
involved.
Function effectively as'a member of a team and prepare a meaningful laboratory
report.

Safety in the Laboratory

Ensuring the safety of personnel and protection of facilities are paramount in any
la boratory experience.

General safety rules

1. Every student must wear Iab coat and shoes (slippers or sandals are totally
prohibited) and student must always be in a good manner.
2. Practice good housekeeping, Make sure all tables and experimental surroundings
are in a clean and organized condition and all tools should be placed in order
before leaving the Iaboratory,
3, All the specific safety precautions in the laboratory must be obeyed.
4. Students should be responslble on the equipments. Do not leave the lab while
apparatus is on,
5. Every student is prohibited from smoking, drinking or eating in the laboratory.
6. Pay attention and be careful when running the experiment to govern the accuracy
of the results and to avoid accidents.
7. Students are not allowed to run experiment after the scheduled time except for
cases where it is ordered by the supervisor and the student is monitored by
lecturer and laboratory technicians.
B. AII Iitters and wastes from the experiment must be thrown away in a dust bin or a
special designated area. Do not throw Iitters and wastes in wash bin or urinal.
9. Do not make noise in the Iaboratory.
1C. Students must familiarize themselves with the Iocation of emergency aids e,g. fire
extinguisher/ emergency shower etc.
11, Any accident must be reported immediately and verbally to Iecturer and/or
laboratory technicians.
ffitI
Attendanee and participation
SEPITRATION PROCESSES LABORATORY II

The nature of laboratory studies is not only the limjted time,

activity intensive but also
Iimited in resources Therefore, attendance at the regulariy
schedulecj cjass sessions is
vital to successfuliy produce the required deliverables. Team members
depend on the
availability of the entire team to maximize the value of the
team's products. in addition
to that, the following rules must be comolied:

1' Students are mandatory to participate in all the ouilined experiments.

students is
considered FArL if they do not attend even one experiment,
Students are also
required to sign an attendance record.
2' Students mtlst come t6 thre Iaboratory 10 minutes earlier
before the experiments
starts, well prepared and organized. To ensure the experiment goes
smoothly,
students are required to read and understand the work procedures
and
experimental theory before the lab hour.
3' Each experiment will take around 3 hours. students
will be divided into several
groups' A supervisor wili conduct the class and
wi{l be assisted by Iab technicians
The time allocation for the experiment is as follows:

,. r it: i lr(.ri -irl-i( ji

ntal procedu re a
weil as identifying the equipments and apparatus needed.
The next 1.5 hrs Students run the experiment
The next t hr Students must complete the lab report
The last 15 min Students clean up the working area and the equrpments
used.

Grading

The final qrade of this course is determined from all graded

objects with weighlng and
grading as follows.

Summatiye as^sessment

\lr.t .'i "art,.ijrrr, ., i,1,liGi .l s

Test
20o/o
Overall Total
100

The date, time and venue of lhe test wijl be announced

once after all the experiments
are compleied.
@MTM SEPARATION PROCESSES LABORATORY II

12. Experimental data must be endorsed by lecturer or laboratory technicians after

completing the experiment.

Safety attire

1.Every student must wear proper safety equipments at all times when running an
experiment. Most of the experiments involve chemicals, high temperature and
pressure. Therefore, safety glasses must be put on to protect the eyes.
2. Safety helmet must be used if students need to climb; e.g. distillation column
to
collect data and record the observation.

Laboratory equipments

1, Students are prohibited from using the experimental equipments before receiving
a comprehensive explanation from lecturer/laboratory assistants. This is not only
dangerous to the students and other lab personnel in the Iaboratory, but can also
damage the equipments.
2. Before using the equipments, make sure of the appropriate and correct power
source and plug for the equipments.
3. Sensitive equipments cannot be moved. Use the equipments in the designated
area,
4. Any damage to the equipment while using it must be reported immediately to the
responsible laboratory technician. Do not try to repair it yourself.
5. Students are forbidden from using damaged equipments,

Disposal of laboratory's wastes

1. Students are held responsible for cleaning the table area, equipments that they
used as well as the laboratory surroundings to avoid hazards to other users.
2. wastes must be properly labeled and disposed in a designated area.

Electricity, gas and others

1. All sources of gas, fuel and gas flow valve must be turned off tighgy before
Ieaving the laboratory and when they are not in use. The cover of a fume
chamber must be lowered to the lowest level.
2. Make sure the right power source is used with the equipment to be
engaged. Equipments which are not in use must be switched off.
3. If students intend to leave an operating equipment, make sure the equipment
can
operate safely' Students also need to inform their absence to the Iaboratory
tech n icia ns.
ryrIHh# SEPARATION PROCESSES LABORATORY II

Assessment of each experiment wiil be based on the foilowing;

@verad"l tea,tn a,ssess"rat€ nt for ea,ch eNrperfun,ent

Identification x System identification sheet

Lab Preparation
Reportxx Experimental sheet
Q&A on lab
preparation report (based on Lab preparation
explanation and l Re po rt)
justification x
Final Reportx* Group report
Professiona Iism x Observatron checklist

*individual assessment
x*team assessment

*xTeam-based Lab work

will be multiplied with a grade adjustment factor from peer
rating to assess students'team working ability. Students have to
submit the peer rating
form after each experiment. otherwise they wiir get a factor of
zero.

Individual assessment for professionalism will be based

on the following attributes:

' Accountability
' Pa rticipation

' Clothing
' Ethrcs
' Safety
ffiKITM SEPARATION PROCESSES LABORATORY II

The Iab reports will be assessed by proportionally weighting performance in the following
catego ries.
-*.$n; ,4.5$elsgp1n,1;11,r:i :frg
e*t:tlri
1 Technical Aspects 5o/o

2 Abstract 7Oo/o

J1 I ntrod uctio n 1Oo/o

4 Literatu re Review/Theory 7Oo/o

5 Methodology !0o/o
6 Results 7Oo/o

7 Discussion 3Oo/o

B Conctusion 10%

9 References 5%

Overa[[Tota1 100%

Lab reports should be submitted not later than 1 week after the experimental work
Students are responsible to submit all lab report on time. Failure to do that will be
penalised 107o per day.
ffiTJTh# SEPARATION PROCESSES LABORATORY II

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Basically, your La'b Report should tell what you did, why you
did it, what you learned
and the significance of your results. The report does
not have to be extremely long. In
fact, the key to writing an excellent report lies in presenting
concisely your response to
the objectives of the project and justifying that response
with appropriate documentation.
The Lab R.eport should consist of the following sections:

1. Title page
This page should include the title of the experiment, experiment
date, submission date,
name of the supervisor, secti6n no/ group no/ name of
the group members.

2. Abstract
The abstract is the report in miniature. It summarizes
the whole report in one, concise
paragraph of about 100-200 words. As distinguished
from the introduction, the abstract
tells the reader what will be done and lays the groundwork.
Aiso, the abstract
summarizes the report itself, not the actual experiment.
Hence, you cannot write the
abstract until after you,ve completed the report.

Before wrlting the abstract, it is often helpful to summarize

each section of the report
(introduction, methods and materials, procedure, results,
discussion, and conclusion) in
one sentence' Then try to arrange this information into
a short paragraph. Remember,
the abstract should be a precise and specific summary.

3, Introduction
Pertinent background and explanatory information about your
experiment must be
presented if your audience is to'connect the
dots'of later sections of your report.
Typically there is both an organizational need and a technical
problem, you should
briefly introduce the purpose of the study, the nature of the technicalso problem, and
argue for this work's importance by putting it in the context
of the industrrai practices or
the state of knowledge. This information emanates from the probiem
statement,
scenario, or other context of the assignment.

4, Literature Review/Theory
The Literature Review and/or Theory section is a brief
review of relevant ideas from the
malor fieid and a more intensive coverage of the specific topic
at hand in yo.,r own
words only pertinent articles or textbook materials relevant to
the assigned topics are
cited' The Iiterature may reveal conflicting views and opinions
on the iopic; these are
included in the review in an unbiased way. -i-he underlying
physical principies, iaws and
governing equations relevant to the problem are presented,
state the assumptions and
iimitations of the theory' Charts, diagrams, and other exhibits may be used
rn
developing and expiaining the theory, especially if they
aid clarity and conciseness. The
relationship between academic/laboratory and rndustrial
perspectives (Connection and
@klthn SEPARATION PROCESSES LABORATORY II

application of concepts from the pilot-process to the real industrial processes) must be
explained.

5. Methodology

Assumption and justification involved while doing the experiment and preparing the
report may also included. Importance and information on precautious/safety aspect of
the experiment may also highlighted and discussed, if any. This rewrite should now
reflect the actual experimental program as implemented by your team, and thus be
consistent with the upcoming Results and Discussion sections.

6, Results

The Results section delivers the evidence that will help answer the questions raised by
the objectives of the investigation, should prepare readers for the more detailed
upcoming discussion, and justify the conclusions that will be drawn next.

Observations, data and calculated results (in consistent units) are often presented best
as graphs or charts, particularly if it will be important to illustrate trends. However,
tables make sense when you need to present accurate data and specific facts or
demonstrate the relationships between numerical and/or descriptive data. Figures and
tables should include - whenever possible - published, theoretical , andfor
model/simulation values available from the literature or produced programmatically,
Tables of raw experimental data are not placed in this section; they are reported in
appendices. Other results that do not relate directly to the upcoming discussion can
either be reported in the Appendix, or by reference to the Lab prep Report. Data are
often summarized or reduced for presentation, Reducing the data allows generalizations
to be made and trends to be pointed out.

Obviously, then, charts and tables must be accompanied by appropriate text. Every
figure or table itself is numbered and supplied with a brief but descriptive tiile or caption.
Build graphics and other visual displays so that, with their accompanying description,
they are self-explanatory. Consult a good reference for guidelines on producing quality
graphs and tables. The Results section text briefly explains how the results were
obtained from the experimental data, the associated quantitative uncertainty (e.g.,
confidence Iimits, standard error, etc.), references to appropriate equations or sample
calculations, and any critical assumptions or approximations made in obtaining the
results. However, best practice in bringing together your exhibits and your words is
accomplished by referring readers to graphics explicitly and telling them what trends to
notice.

7. Discussion

If the Resultssection delivers the evidence, the Discussion section makes the case in
court. In the Discussion section, you explain what your experimental results mean by
relating them to the concepts and ideas presented in the Introduction and Literature
Review/Theory sections.
ffi,tIHh# SEPARATION PROCESSES LABORATORY II

There are many questions that could be answered in this section

so you should not limit
yourself to those offered here as examples. Answer the questions
that make most sense
for your work.

" Do the results agree with theory, with the work of others, with
models/simulation? If so, how? If not, why not? Can the disagreement
be
explained?
. What are the most probable sources of experimental error and have these
affected your ability to draw conclusions? How might these errors
have been
reduced or eliminated?
' Did your results reveal problems with the experimental plan, method,
or
equipment? How might these be improved?
, Were your assumptions suspect or reliable?
' what definite conclusions can you draw from your results? what conclusions
are
more specu Iative?
" what implications do your results have on theory and current industrial practices?
' What questions remain unanswered? What questions should
be answered next?

In this section, you may also criticize the Iab experiment and make
recommendations or
improvement' Such criticisms and recommendations, however,
should focus on the Iab
as a learning experience; mere complaints about faulty
equipment or amount of time
spent are not appropriate.

8. Conclusion

Draw conclusion from the results and discussion that answer the
objectives of the
ment' Then go on to explain your conclusions that summarizes and
experi
reflects the
resuits and discussion.

9. Nomenclature

AII symbols and acronyms used in the report and rts appendices
must be listed and
defined in a Nomenclature section with the consistent set
of units used for
calculation/reporting of resuits. Symbols are arranged in alphabetical
order, Latin terms
(e.9,, a, b, D, Re, pr, etc.) first, followed by Greek (e.g., o, p, p,
etc.), and finally
subscripts (e,g., i, j, k, etc.)^ Greek and subscript sets are
headed by the tiLles.Greek,
and'Subscri pts'.

In addition to the Nomenclature section properi introduce these symbols

where they first
appear usinq either running text or a iist set off from ihe
running text. If a dozen or
fewer symbols are used jn this report, you may rely on the in-text
introduction of
symbols and acronyms alone and forego a separate Nomenciature
section altogether.

lO.References

rhe Literature Cited section inclr,rdes all references from which materiai
was taken lt does not include materials consulted but not cited,
in this report
citations iisted in any appendix document (e.g., citing of handbooks
It does include
properties data have been taken). A report without
from which
ANy cited iiterature is typicaliy not a
ffiTJTM II
SEPARATION PROCESSES LABORATORY

credible piece of work. Citing the literature typically strengthens any case you are
making in your own reporting.

The in-text citations themselves should give the page number(s) relevant to the actual
material cited. The in-text citation plus the full reference in the Literature Cited section
make it possible for the reader to find the material.

l l.Appendices

Appendices may include raw data, calculations, graphs, and other quantitative materials
that were part of the experiment, but not reported in any of the above sections. Refer to
each appendix at the approp"riate point (or points) in your report. For example, at the
end of your results section, you might have the note, See Appendix A: Raw Data Chart.

Adapted from: Unit operations Laboratory syllabus, cain Department of chemical Engineering,
Louisiana state
Universtty; Fluid Mechanics Laboratory, Polymer Engineering Laboratory 2, Faculty of chemical
Engineering,
Unive.siti Teknologi Malaysia.
ffi,tTth# SEPARATION PROCESSES LABORATORY II

r S', ))i! i.: )ii l,r'i-:lli i tilll[..]..\.',- --

EXPERIMENT 1: SIEVING

EXPERiMENT 2: FLU]DJZED BED

EXPER]MENT 3: VACUUM FILTRATION

EXPER]MENT 4: TRAY DRYER

EXPERIMENT 5: SPRAY DRYER

EXPERIMENT 6: CL]MB]NG FILM EVAPORATION

EXPER]MENT 7: VAPOU R-LIQU]D EQUILIBRIUM
 UTM
UNIVERSITI TEKNOLOGl MALAYSIA
SEPARATION PROCESSES LABORATORY II

ffiXPFRTMENT T
srF'wuruG

Backgrou.rad sf Exp,eri.noent

Sieving refers to the separation of a mixture of particles of different sizes using sieves
each with a uniform sized opening. Standard sieves of specified opening sizes are
used.
Sieves are stacked with the sieve with the largest opening on the top and the material
is
separated into fractions by shaking, The material between two sieves is smaller
than the
upper sieve opening but larger than the smaller sieve opening.

Many natural and manufactuied materials occur in a disperse form, which means
that it
consist of differently shaped and sized particles. The particle size distribution, i,e.
the
number of particles of different sizes, is responsible for the determination of important
physical and chemical proper[ies such as:

' mechanical bulk behavior

. surface reaction

' m iscibility
' filtrationproperties
' co nd u ctivity

This list could be continued at great Iength, The examples clearly show how important
it
is to have knowledge of the particle distribution, particularly within the context
of quality
assurance in the production of bulk goods. If the partlcle distribution changes during
the
manufacturing process then the quality of the finished product will also change,
only a
continuous monitoring of the particle size distribution can guarantee a constant product
quality.

Objective of Experiment

In this experiment, students will determine the particle distribution using sieving method,

Scopes of Experiment

Given a sample of particulate solid, you are assigned to conduct sieving experiment
using sieve shaker with designated dimension (with mesh openings that reveal particle
distribution at critical sizes). if the particle range of material representing feed to
a
screen or product from a crusher is wide, you have to use a large sample (from
500 to
1,000 grams). If the material is finely ground, use a smaller sample of 25
to 100 grams.
From this experiment, you should determine the particle distribution. The
steps required
must be repeated at Ieast three times to get more accurate result.
 UTM
UNIVEHSITI TEKNOLOGI MALAYSIA
SEPARATION PROCESSES LABORATORY II
Description of Experiment

Fa rticle size determi nation methods

There are different methods in determining the particie distribution

(Figure 1.1). The
choice of a particuiar method depends primarily on the
dispersion status, i,e. on the
degree of fineness of the sample.

Particle 5 ize Determ in ation Metho ds

Automatic im agi lnal,rs b (El:ctror h,licr,r;.rp+)

C : nirifug:l ; edim tnlation

tl DU iie r t-' (, U frtr i

G ravim elrir ; edim antstigrr

P hol0.optib:i m eihrrd

U ltres o nic

Figure 1'1: Particle Size Determination Methods (Retsch; Solution

in Milling & Sieving,
15'" Dec 2010)

The oldest and best-known method is particle size determination

by sieve analysis. The
particle size distribution is defined via the mass or
volume. Sieve analysis used to divide
the granular material into size fractions and then to determine
the weight of these
fractions' in this way a relative{y broad partlcle size spectrum
can be analyzed quickly
and reliably (Retsch; Solution in Milling & Sieving, 15rh Dec
2010),
ffiMTM SEPARATION PROCESSES LABORATORY II

(a) (b)
Figure 1,2: (a) Sieve shaker (b) Sieves with different mesh openings (Retsch; Solution
in Milling & Sieving, 15th Dec 2010)

Experimental Proced ures

Performing a Sieve Analysis

You can begin your particle size distribution analysis after you properly collect, prepare
and size a sample. Select test sieves with mesh openings that reveal particle distribution
at critical sizes. These are usually stated in a product specification or determined by
material processing requirements.

To perform the analysis, do the following:

1. Siack the sieves on top of each other with the coarsest (largest opening) on the
top of the stack.
2. Put the bottom pan under the finest (smallest) opening sieve. This pan collects
"fine" material that passes through the last one,
)J. Use a Iaboratory scale (accurate to.1 gram)
to weigh an empty container (such
as an extra empty bottom pan) and establish the tare weight.
4. Weigh the sample material.
5. Empty the sample into the top of the stack. Make sure you do not overload the
surface as this causes "blinding" or blocking of the openings.
6. Put the stack into the sieve shaker.
7. Place a cover on the top of the stack" (If do not have the cover, you need to
determine the sieving loss)
B. i'v'lake sure the stack is securely in place.
9. Set the proper length of time to agitate the materral.
10.Turn on the shaker and run the test.
ffi[JThf, SEPARATION PROCESSES LABORATORY II

11'After the shaker stops, empty the material from the coarsest sieve
into the empty
container that you weighed in step (3), Use a soft bristle brush
to gengy brush
the underside of the sieve to remove ail of the particres.
12'Tap the side of the frame with the handle of the brush to clean
the remainrng
material from the sieve.
13' Weigh the contents in the part to the nearest 1/10 gram
and record the data.
14. Return the material to its original sample container,
15'Repeat steps 11 through 14, using the container referenced
in step (3) for each
sieve, including the fine material in the bottom pan,
16'Total the weights to make sure the sum of the retained material
and the material
in the bottom pan is as close as possible to the original weight. check
your
specification for allowable variation.
17' Divide the weight obtained from each sieve by the weight
of the original sample.
Record the percentage for each sieve.
18. Calculate and record the cumurative percentages
as required.
19, Repeat all the steps above for 3 times.

Experirnental Resul,t

Based on the above procedures, you need to identify

what kind of data you should
extract from the experimental work. Then, ail the data must
be recorded in a table.
Example of the tabie of experimental result is as Table 1.1:

Table 1.1: Experimental result of sieving

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 II
@MHM
SEPARATION PROCESSES LABORATORY

Result and Discussion

Questions

The following questions must be explained explicitly in the result and discussron.

1. What is the fractions, p3 of the samples in each class of particle size. (This can be
shown graphically in bar charts or histogram). Sample of the graph is as follows:

rl '.
I rri. I
Q::i3ri

9!
8[

ui
50o/o

:lu

30

2S

r*

ir.ti]O 0.trr1 0.1.?5 +0.2tO0.5 j (l (:i;

x.. -i-1.189rtnr x[mm]
Figure 1.3: Fractiors, p3 against the class of particle size (nominal sieve mesh), x

2. Sorting can be expressed by various statistical methods, The simplest of these is

the measurement of the central tendency of which there are three commonly
used parameters: the median, the mode, and the mean. Therefore, based on
your answer in (1), what is the median, the mode and the mean of your results
and how does the figure reflect the sieve analysis.

3' Plot the cumulative percentage of particle size that less than the mean particle
size, Dpi for each mesh opening of the sieve. Then, determine the particle size at
the cumulative percentage of \60/o, 5Oo/o and B4o/o.

4. Calculate the particle size distribution using the following equation:

Ps+ . Pro
Particle Distribution .
2
 UThd
UNIyEBSITi TEKNoLocr Nnllistn
SEPI\RATION PROCESSES LABORATORY II

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B-ackg,rou,rld of Exp€riffl,erlt
The upward flow of fluid through a bed of particles
is a situation encountered both rn nature, as
with the natural movement of ground wateT, crude petroreum
media' and in industrial operations such as backwashing
or naturai gas, through porous
firters, ion* exchange processes/
extraction of soiuble components from raw materials
and for cerlain types of chemical reactor. It
well known that if the particles are loosely packed is
and Lhe pressure drop due to the flow through
the bed is equivalent to the weight of the bed, the phenomenon
of fluidization occurs. The fluidized
state occurs naturally is so-called'quick sand'and
industrially, use is made of the high rate of
solids mixing that accompanies'fluidization for various
operations such as drying, coating, heat
transfer and chemical reaction.

This equipment is designed to allow the study

of the characteristics of flow through both fixed
fluidized bed of solid particles. Although the and
majority of fixed and fluidized bed situatrons
encountered by practicing engineers are
three dimensional, in order that students can readily
observe the important phenomenon of bubbling
that occurs in gas-solid systems when the gas
velocity is in the excess of that required for fluidization.
The transparent walls allow studies to be
made of bubble behaviour in the gas_solid system.

Objective of Experirnent

1n this experiment, students are required to study

the behavlour of fluidization.

Scopes of Experiment

In this experiment, you have to investigate the principles

of fluidization of fine sand
using fluidized bed' For different air flow rate
supplied to the system, you need to further
study the characteristics of fluidized bed such
as the thickness and the condition of
fluidized bed formed, and also the pressure
drop.

Description of Experiment

Many important industrial processes rely upon

intimate contact between a fiuid (liquid or
gas) and a granular material. In eariy applications,
the fluid flowed through a statrc bed
of granules supported on a grid provided the material
is suitable, greai improvement in
mixinq and contact is achieved if the granule size properly
is matched to the upward
velocity of the fluid' The particles of material
wili be supported by the drag forces and
the bed is saici to be "fluidized,,. The fluidized beds
show lollowing Iiquid or fiuid like
p ro p erti es.

The pr-incipie of opei-ation of fluidized systems

are based on the fact that if a gas is
alloweci to tlow through a bed of particulate
solids at verocity greater than the setling
velocity of the particles and less than the terminal
verocity for pneumatic conveyrng and
equal to the minimum velocity of fluidization (V
mr), the solids get partially suspended in
ffiTJTM II
SEPARATION PROCESSES LABORATORY

the stream of upward moving gas. The gas stream negates the gravitational pull due to
weight of particles to enable the suspended state of the solid.

The resultant mixture of solids and gas behave like a liquid and thus righily solids are
called Fluidized. The solid particles are continually caught up in eddies and fall back in a
random boiling motion so that each fluidized particle is surrounded by the gas stream for
efficient drying or granulation or coating purpose. In the process of fluidization there
occurs an intense mixing between the solids or gas resulting in uniform condition of
temperature/ composition and particle size distribution throughout the bed.

A mass of finely divided solids is transformed into a fluidized bed by lifting action of gas
passing through it. Thus threE stages can be identified in the process of fluidizing a bed
of solids basing on the velocity of gas flow through it. They includer

' Fixed bed or Static Bed

. Expanded bed or particulate fluidization.
. Mobilized bed

As shown in Figure 2,1 below, the velocity of the fluid through the bed opposite to the
direction of gravity determines whether the bed is fixed, expanded, or is swept out. This
Ied to the development of the concept of minimum fluidization velocity (y *r) at which
the bed just begins to fluidize. Thus the primary concern is to measure and optimize
the V ,6for efficient fluidization,

rT
tfr

(a) Slow flow rate (b) Intermediate flow rate (c) High flow rate
Figure 2.1: Fixed, Fluidized, and Mobilized beds.

The fixed bed (a) occurs when the approach velocity or superficial velocity, ( l,/o ) , is
much smaller than the minimized fluidization velocity,( Y
-r).The fluidized bed (b)
occurs when the approach velocity is intermediate between the minimum fluidization
velocity and the terminal velocity. The pneumatically mobilized bed (c) occurs when the
approach velocity is much greater than the particle terminal velocity, (U,).
ryrJHhn SEPARATION PROCESSES LABORATORY II

Experirnental Result

Based on the above objective, you need to identify the

required data to investrgate the
fluidization process. Then, all the data must be recorded in a
tabie.

Example of the table of experimental result is as Table 2.1;

Tabl,e 2,1: Experimental result of fluidization

AEr" f0orrur l"ateo liEngeEcmess of tEne Fr.essune drop, @hsenvatnom
t/ mtn hed c-orii liEme sar,ad. ntnOH2@ (ffiundrzed: heci of
.;lln i:ifrire ,sAl{,ire ,

Result and Discussion

Questions

The following questions must be explained expiicitly in the

result and discussion.
1' PIot a graph of (log) pressure drop versus (log) air flow
rate. Explain the curve
obtained from the experimental resuit based on the condition
of fluidized bed of
fine sand observed during the experimental work.

2' Determine the fluidization point and what is the air flow
rate at the fluidization
poi nt?

3' calculate the bed void fraction, ay of the fluidized bed of the
frne sand.
 SEPARATION PROCESSES LABORATORY II

EX PFRXr.uf FNT *
W A( HJ[.uM FHh trRA E E (lft
This experiment is conducted through pBL method,

The objectives to be achieved by this experiment are:

' To characterize the flow through the cake in a simple Iaboratory test
' To calculate G and R, at different vacuum pressures (100, 200, 300, 400 mmHg)
. Material: Calcium carbonate (CaCO3)

Write a complete report which would lead to achievement of all the stated objectives and
answer all the following questions.

Questions

The following questions must be explained explicitly in the result and discussion,

1, Plot a graph of Vp versus time and calculate the filtrate flow.

2. Plot a graph of t/ Vr versus Vp for every vacuum pressure. From the graph,
determine the filtration constant.

3. Calculate the specific resistance of the filter cake and the specific resistance of
the medium,

4. Discuss the relationship of between the specific resistance of the filter cake and
the vacuum pressure; and between the specific resistance of the medium and the
vacuum pressure, Explain the effect of vacuum pressure on both parameters.
 UTM
UNIVERSITI TEKNOLOGI MALAYSIA
SEPARATION PROCESSES LABORATORY II

;F-X iD:1E1*. t'iiiviil irrv :.1

,R,,4 ' rlR r' ; o

BackE.ror,r nd of Experinrent

The term "drying" is a reiative one, and simply means that there
is a further reduction in
the moisture content from some initiai level provided by mechanical dewatering
to some
acceptable lower level. For example, moisture content of 1o-20%
by volume would
normally allow particles to flow freely, yet suppress dust formation,
The necessity
drying may be to make a product suitable for sale or for subsequent processing, for
e.g.
example paint pigments; of for subsequent processing, e.g in pyrometallurgical
operations

when a solid dries, two fundamental and simurtaneous processes

occur:

' Heat is transferred to evaporate liquid;

' Mass is transferred as a liquid or vapor within the solid and
as a vapor from the
su rfa ce.

These factors governing the rates of these processes determine

the drying rate.
Commerciai drying operations may utilize heat transfer by
convection, conduction,
radiation, or a combination of these. Industrial dryers differ fundamentally
methods of heat transfer employed. However, irrespective of
by the
the mode of heat transfer,
heat must flow to the outer surface and then into the interior
of the solid,

Careful consideration of many factors is necessary in the final

selection of the most
suitable iype of dryer for a particular application. Some of these
factors are:

' Properties of the material being handled

, Drying characteristics of the material
. Flow of the material to and from the dryer
" Product qualities
. Recovery problems
' Facilities availabre at the site of the proposed instariation.

Objective of Experiment

in this experiment, students wili be exposed to the operation of tray

dryer r,vhereby they
are required to study the drying behaviour of a non-porous sorid.

Scopes of Experiment

After dryinq the solid experimentally using tray dryer, you need to
analyse the
experimentai data relating moisLure content to time and lt
should be represented by
typicai dryinq curves. Besides, the study of drying behaviour
can be carried out further
by determining the drying i-ate of the soiid and also by calculating
ihe heat and mass
transfer coefficient during the constant rate oeriorJ.
 SEPARATION PROCESSES LABORATORY II
ffiTJHM
Description of Experiment

When a solid is dried experimentally, data are usually obtained relating moisture content
to time. Consider the drying of a non-porous, insoluble material such as sand or rice in a
tray. The surface of the rice is exposed to a drying medium such as hot dry air passing
over the surface. Figure 4,1 shows the typical drying curves in investigating the drying
behaviour of a substance.

c
+o o
c
o 6ry
LE
q) Ol ,
L .L
f lo)
+ (J
o o
o
2
I
X
E

Tlme (mlns) Molstur^e Conlent

* X| - equilibriu m moisture content

Figure 4.1: The typical drying curves

To experimentally determine the rate of drying for a given material, a sample is usually
placed on a tray. If it is a solid material it should fill the tray so that only the top surface
is exposed to the drying air stream, By suspending the tray from a balance in a cabinet
or duct through which the air is flowing, the loss in weight of moisture during drying can
be determined at different time intervals without interrupting the operation. The velocity,
humidity, temperature, and direction of the air should be the same and constant to
simulate drying under constant drying conditions. In this course, a tray dryer as shown
in Figure 4.2 is used to perform this experimental work.

Fig,ure 4.2; Tray dryer

ryIJHM
The Drying Curve
SEPARATION PROCESSES LABORATORY II

For each and every product, there is a representatrve curve that descri
bes the drying
characteristics for that product at specific temperature, velocity and pressure
conditjons.
This curve is referred to as the drying curve for a specific product.
Variations in the
cuTVe will occur principally in rate relative to carrier
velocity and temperature. The curve
is extremely valuable in understanding idiosyncrasies associated with
the drying of each
unique product.

In discussing the drying process, typically, there two fundamental temperatures

involved.
The dry bulb temperature is the temperature of a body or air as
measured with a
conventional thermometer. In process applications, it is the process
control set point of a
dryer' It is also referred to ds just "temperature". Meanwhile, wet bulb
temperature is
different' It is called "wet" because a permeable membrane such as wet gauze
is used in
coniunction with a regular thermometer to obtain the reading. The gauze
is wrapped
around the bulb of the thermometer and inserted into the gas stream.
Because the water
is evaporating off the gauze in the gas stream, evaporative cooling ensures
that the
temperature is lower than a dry bulb thermometer in the same gas physically
stream.
obtaining this reading is tricky because the reading is meaningfui only
at a constant rate
of evaporation, Too much or too little water wlll affect the reading, and
it takes practice
to obtain the correct value. The dry and wet bulb temperatures are fundamentals
in
defining the properties of the air.

t!
o +
o.
E
.o Exha irst Ierrrperature
o
Counter' o
;fu G
0, ?
G
G,
=
g)
'i Prodtrct
peiarlure
o Te nr

fime

Figure 4'3: Different phases in drying processes; initiar period, constant rate
period and
falling rate period. (process Heating; The Drying Curve, 15rh Dec
2010)

Figure 4'3 represents a typical drying curve for virtually any product. Dryrng occurs
in
three different periods, or phases, which can be clearly defined. The
first phase, or
initial period, is where sensibie heat is transferred to the product and
the contained
moisture' This is the heating up of the product from the inlet condition
to the Drocess
 UTM
UNIVERSITI TEKNOLOGI MALAYSIA
SEPARATION PROCESSES LABORATORY II

condition, which enables the subsequent processes to take place^ In some instances,
pre-processing can reduce or eliminate this phase. For example, if the feed material is

coming from a reactor or if the feed is preheated by a source of waste energy, the inlet
condition of the material will already be at a raised temperature. The rate of
evaporation increases dramatically during this period with mostly free moisture being
removed,

During the second phase, or constant rate period, free moisture persists on the surfaces
and the rate of evaporation alters very Iittle as the moisture content reduces. During this
period, drying rates are high, and higher inlet air temperatures than in subsequent
drying stages can be used without detrimental effect to the product. There is a gradual
and relatively small increise in the product temperature during this period.
Interestingly, a common occurrence ls that the time scale of the constant rate period
may determine and affect the rate of drying in the next phase, The third phase, or
falling rate period, is the phase during which migration of moisture from the inner
interstices of each particle to the outer surface becomes the Iimiting factor that reduces
the drying rate,

Experimental Procedures

The equipment setup of this experiment is shown in Figure 4.

1' Weigh the cooked rice before adding some water, The rice should be removed
from the container and drained excess .'free water,,.
2' Distribute about 1000 g of the wet rice between all four trays, The initial moisture
content should be more than 10o/o. The total weight of the wet rice should be
noted before drying commences,
3, At some arbitrary time (t=0), switch on and set the fan speed control to mid-
position (5) and the heater power control to position B, letting them remain
constant th roughout the experiment.
4. Wait until the dryer reaches a steady state temperature.
5' Record the wet and dry bulb temperatures at the three locations (inlet air
position, and both before and after the drying trays, see positions 1,2 and 3
shown in Figure 4.4) for time = 0 s and record the air velocity.
6. While the material is being dried, record the following:
a' The total weight of rice in the trays at regular time intervals until drying is
complete, i,e., the weight remains constant. (At the beginning use short time
intervals since the drying is fast and then make it Iong as the drying becomes
slow).
b. The wet and dry bulb temperatures at the three Iocations and the air velocity.
 SEPARATION PROCESSES LABORATORY II
ffiTTHhf,
Heater power balance
contr'oi Heaier Dtgrral
F lap anemometen
,A1r'
--*----* Alr
------------>
lnlet ? ouilet
Door / \Tr^ags
Fan speed
control
Power
outlet

Figure 4.4: Schematic diagram of tray dryer

Experirm erl.ta I Resu lt

Based on the above procedures, you can plan the time intervals
for the data recording. It
is recommended for you to record the data for every two minutes
within the first 1o
rninutes, then you can increase the time interval as the drying progresses. you
need to
record the experimental result until the process is complete
i,e, the weight is constant.

Example of the table of experimental result is shown as Table

4.1 (you can modrfy the
table according to your needs):
 o o
]E 1U .i'

^;
- I

f; tto
-r+Gt
El -r :f
-6',+
oq
oFr
ils
,+=
!o
o
E{
-r
EJF
cEr
o
Er

7
..:
@
')

q\-{
=F4
tf tt tf ,t * *
IJJ N UJ N ts
EH
6

=<

{g
I
ri
F
l:
m
x
E
o
=.
3
o
:l
-l
OJ

T
o
c
=
,b
-
f
OJ

o-
-
e0
o
f
a
m
!
NJ
hJ F
l{
o
h z
!
v
o
o
m
o
V,
m
a
E
o
F
-5
o
v
!(
w
rymJthfl
SEPARATION PROCESSES LABORATORY II

Results and Discnssion

Qwestions

The following questions must be explained explicitly in the result and

discussion.

1' Using the weights measured during the experiment calculate ihe dry basis
moisture content of the sampre at given varues of time;

X=
W-Wr kg total water
*, kg dry solid
.
W is the weight of the wet solid (total water+dry solid) and W. is the
weight of
the dry solid

2. PIot the drying curve (moisture content versus time)

3' Calculate the drying rate aL given values of time. The drying rate
R is calculated
for each point by:

,,
r\-
W, dX
Adt
4' Plot the drying rate curve (drying rate versus moisture content).

5' From the drying rate curve estimate the drying rate within the constant
rate
period, R. and the criticai moisture content, X..

6' Calcuiate the heat and mass transfer coefficients during the constant
rate period.
7 ' Estimate the time of drying during the constant-rate period and the
falling period
and hence calculate the total drying time. Compare your results with the
experimentally measured one.
 TM
IEKNOLOGI MALAYSIA
SEPARATION PROCESSES LABORATORY II

ffixpFffi"srvlFts ?' 5
sFmA * imft wFffi

Background of Experiment

Spray drying is a very widely applied, technical method used to dry aqueous or organic
solutions, emulsions etc., in industrial chemistry and food industry. Dry milk powder,
detergents and dyes are just a few spray dried products currently available. Spray drying
can be used to preserve food or simply as a quick drying method. It also provides the
advantage of weight and volume reduction. Ii is the transformation of feed from a fluid
state into a dried particulate form by spraying the feed into a hot drying medium.
intensive research and development during the last two decades has resulted in spray
drying becoming a highly competitive means of drying a wide variety of products. The
range of product applications continues to expand, so that today spray drying has
connections with many things we use daily.

The spray drying process transforms fluid feed into a dried product in a single operation.
Basically, spray drying is accomplished by atomizing feed liquid into a drying chamber
through a rotating wheel or nozzle, where the small droplets are subjected to a stream of
hot air and converted to powder particles as a result of moisture evaporation. The
resulting rapid evaporation maintains a Iow droplet temperature so that high drying air
temperatures can be applied without affecting the product. The drying proceeds until the
desired moisture level in the products is reached.

As the powder is discharged from the drying chamber, it is passed through a powder/air
separator and collected for packaging. Most spray dryers are equipped for primary
powder collection at efficiency of about 99.5o/o, and most can be supplied with
secondary
collection equipment if necessary.

Objective of Experiment

In this experiment, students will study the process of spray drying which is applied to dry
aqueous or organic solutions, emulsion, etc.

Scopes of Experiment

In this experiment, you need to study spray drying process including its principles of
transformation of feed from liquid state into a dried particulate form, the application
of
the process, the uses of spray dryer and type of spray dryers. you have to produce your
own product from the spray dryer, then the density of the product obtained from the
experiment should be compared to the standard density. You need to investigate
the
instrument settings, namely inlet temperature, feed rate, spray air flow in order to
further study the product parameters such as temperature Ioad, final humidity, particle
size and yieid' Besides, you can also compare the density of the product obtained in
ihis
experiment to the standard density.
ryHHhfl SEPARATION PROCESSES LABORATORY II

Description of Experirnent

Spray drying is suited for most real or colloidal solutions, for emulsions and
dispersions
as long as the dried product behaves like a solid.

Figure 5"1: Spray drying of inorganic or organic product (BUcHI Labortechnik AG,
zoo2)
As shown in Figure 5.1, an aqueous solution of the product (A) is dispersed into
fine
droplets (B) using a two fluid nozzle. The soivent evaporates immediately surrounding
the product rn a vapour cloud that protects the product from thermal load. As soon
as
the criticai concentration is exceeded, nucleation starts forming a solid shell. After
the
solvent is dried away from the surface, the interface moves into the core (second
step of
drying) The final product (c) is a fine, amorphous or crystallized rnaterial.
Spraying
highly concentrated solution resurts in a more porous final product.

In principal, the spray drying process is dependent upon the solution flow rate, solution
temperature, air flow rate, air temperature and feed concentration. These instrument
settings are in a combined system influencing the product parameters; temperature
load,
final humidity, particle size and yield. The time of drying the droplets is very short jn
comparison with most other drying processes, Low product temperature and
short drying
time allow spray drying of very heat-sensitive products. The optimisation of instrument
settings is usually made in trial and error process. Some initial conditions can
be found in
the application database for equal or similar products.

Spray drying is used to dry pharmaceuticals, foods, dairy products, blood plasma,
numerous organic and inorganic chemicals, ceramic powders, detergents and
other
products' The application depends on the kind of product used, such
as viscosity, density,
additives etc Therefore, the given parameters cannot precisely be overtaken.
Table 5.1,
Table 5.2, Table 5.3 and Tabie 5.4 show some appllcation of spray dryinq process.
 SEPARATION PROCESSES LABORATORY II

Table 5,1: Foodstuffs (BUCHI Labortechnik AG, 2002)

Prsduet lnlet oC Outlet "C Spray concentra*ion yo

Baby food 160 95 40

Beer 180 108
Casein '150 90 6
Yeast o( Ar-
Jri 60
Krill lBO BO 10
Lactose 160 105 JU
Low-fat nrilk 174 102 50
Corn starch 130 70 40
Mitk 110 70 15
Whey 180 BO 6 /45
Soyabean extract (suspension) 130 75 BO
Tofu '1.10
60 17

Table 5.2: Aromas, cosmetics, cleaners and detergents (BUCHI Labortechnik AG, ZOOZ)
Froduct lnlet "C Outlet "G Spray conceRtration %
Valerian extract 150 100 /3
Beer concentrate 150 110 30-40
Chicory extract 130 75 .1.1
Pine bark extract 19n aq
Chestnut extract 200 130 20
Metal soap 165 122 60
Microfoam beads 160 14
'1

Sodium citrate .]60 g0 20

3

Olive leaf extract _ iS0 90 36

Liquorice extract 100 75 JO
Detergent 200 1 10 40
Fahric softener 1?5 7c CCI

Xanthane mixture I'JU 70

Zeolite 180 120 10

Table 5,3: Medical and pharmaceutical products (BUCHI Labortechnik AG, ZOOZ)
Flor{rret }r*et "G Outlet o@ Sprfly
a.l*irraaiilrtraaiirua oA
Albumirr I10 60
Bo 60 ---- j-S -
Bloodplasrna-__ - lBL 100 U
Dexiran 1i;A r on
^^
Enzymes / coenzvmes _ B0 55
trr"t"r"-rr,i." ru ---go---37.- 12

Galactornannan 2AA ill) 5

EAatin capsub BO 20
GlLrcoseramin@-- l3o BO 10
Mannitol with enzvnres -_ 100 55 t5
Uomilnation vaccines I g0 140
Organ *rtru"i
1 : 0,43 _ 1S0 BB 11
Penticles 110 70 2
Vtamin A + /
oelatin-emrrlsion
E 100 (r-
Cell suspension (bacteria cultures) 90 60 ca.50
ryIJTM SEPARATION PROCESSES LABORATORY II

Table 5.4: Chemical products (BUCHI Labortechnik AG, ZOOZ)

,.-.:biirn carcr,naie ')21 iir:r ir_i

'L,t-, r

l iit. ll' I i

l!i- ,irl :iir

:,!i '1i
i r-{[ r l-l

I t'r-
a.I,' iq
r,r. ":-
,:Li
lEIl' 'i!rj ,,.-r

jLlL: Ii',l-r

Experimental Result

In this experlment, you need to identify what kind of data that

should be extracted from
the experimental work. Ail the data must be recorded
in a tabre.

Before you run ihe experiment, make sure the

weight of beaker, inlet air temperature
and outlet temperature are recorded. if possible,
during the process, you are required to
record the inside temperature of the spray dryer at
steady state condition and the
pressure of the compressed air supplied to the
atomrzer. Then, after completing the
experimental work, record the total ttme requrred
for the drying process and weigh the
collected pariiculate sample,
ffiTJHM II
SEPARATION PROCESSES LABORATORY

Example of the table of experimental result is shown as Table 5,5, Table 5.6, and Table
5.7:

Tab|e 5,5: Experimental result for calculation of particulate Density

Eaka Fop' Caler*patron.; raf par"tfre,r.lIate Senscty
Total weight, g
Weight of beaker, g
Weight of sample, g
Standard volume (Vq), cm 6.28
Volume of sample cell (Vs), cm 77.67
Total drying tirhe, min

Tarb'le 5.6: Expgrimental result of inlet and ouilet temperature

'&perattiiom state __]EF!gt iie!1 peF,aEr*re n(, ,CIuthet |e*peuuti*0.e, fE

During experiment
After experiment

Table 5,7: Experimental result of pressure, volume of particular powder and density of
particulate powder
Eata #3 #,'A #3
P1
P2
VP
Density of particulate
powder

Where;

Vp = Volume of particulate powder, cm3

Vn = Standard volume, cm3
Vc =Volume of sample cell, cm3
Pr = Pressure; after applying pressure on the standard density
Pz = Pressure; after taking V6 into account
ry,HHhf,
SEPARATION PROCESSES LABORATORY II

Results and Discussion

Q,uestions

The following questions must be explained explicitly in the result

and discussion.

1' Draw the process block diagram (PBD) and process flow diagram
(pFD) for the
entire spray drying system. Explained the process thoroughly.

2' Using the equation below, calculate the volume of particulate powder
obtained in
this experiment, and then determine its density. Compare the calculate
density
and the standard valu6, and discuss the difference.

VD Pi
'V'I
]iP, I
I

3' Using the temperature measured during the experiment, calculate the
performance of spray drying which is measured in terms of thermal efficiency. If
the drying process is assumed to be adiabatic, that is, the heat Ioss is
negligible;
the overall thermar efficiency (roue,ar) can be approximated to the
reiation;

I overar = I :t- L- t)* , oo n

l lA; l" )

Where Ta1 and Ta6 El-€ the inlet and outlet air temperatures, respectiveiy
and T-
is the ambient air temperature.

4' What kind of modification of the existing system would you suggest
to increase
the recovery percentage of product?
 UTM
UNIVEBSITI TEKNOLOGI MALAYSIA
SEPARATION PROCESSES LABORATORY II

trXPERTfuTHNT 6
E,T.SfiWMBil*G FSLM EWAPffiRA TEffiFU

This expe'ri rment is es.ndruleted' th+o ugrh FB{L n*,e&kr.od,

The objectives to be achieved by this experiment are:

' To study the effect of operating temperature on the concentration profile of sugar
solution.
' To study the effect of feed flowrate to the final concentration of sugar solution,

Design your own methodololies and write a complete report which would lead to
achievement of all the stated objectives.
 UTM
UNIVEBSITI TEKNOLOGI MALAY'IA
SEPARATION PROCESSES LABORATORY II

rF X i,FrlF{R titl{\lfiiFthl;i'; i
,, 4rP'(,);r.],iR, : ,-Jrr,.j I,,l ) Fr.-),t r ,,tB.:R i ,ht4t

Background of Experinrent

Vapour-liquid equilibrium are the fundamental properties whose

knowledge is required,
for example, in the design of separation columns in chemical industries.
Many
experiments are necessary to obtain such equilibrium data,
at Ieast for binary
where non-idealities in both phases must be determined. Thereforesystems,
further
improvements to theoretical models for describing and predicting
these non-idealities are
ind ispensa ble.

At low pressure, devtations from ideal behaviour are due mainly to

the liquid phase, The
association of one or more components in a Iiquid mixture
and the chemrcal forces due to
electrical charge exchange between an associating and an
active compound influence
strongly the excess properties of associated soluiions and the fluid phase
equilibrium.
These effects are in many cases stronger than those
due to physicar forces.

Obieetive of Experiment

The objective of this experiment is to produce vapour-liquid

equilibrium at atmosphere
pressure and to measure equilibrium temperatures
and compositions.

Scopes of Experiment

In this experiment, a mixture of methanor - water wiil be used. From

the experimentai
result in terms of refractive index and the boiling point for different
composrtion, you
need to produce a graph of vapour-liquid equilibrium for
the mixture of methanoi - water.

Description of Experiment

In the analysis of vapour-liquid equilibrium diagram, we shall consider

only 2-component
mixture, e'g' A (more volatile) and B (less volatile). Two types
equilibrium diagrams are widely used to represent data for two-cornponent
of vapour-liquid
(binary)
systems' The first is a "temperature versus x and y" diagram (Txy)
phase diaqram' The x ierm represents the liquld
or it is cailed as
composition, usuaily expressed in term.s
of mole fraction. The y term represents the vapour composition.

The second diagram is a plot of x versus y. This

diagram is also known as equrlibrium
curve' These types of dlagrams are generated at a constant pressure.
Since the pressure
in a distillation coiumn ls relatively constant in most columns (the
exception is vacuum
distillation, in which the pressures at the top and bottom are
significantly different in
terms of absolute pressure level), a t=xy diagram, and an
xy diagram are convenient for
the analysis of binary distillation systems. The Fig ure 7.1 below
shows a constant
pressure phase diagram for an ideal solution (one
that obey Raoult,s Law).
 SEPARATION PROCESSES LABORATORY II
@KIHM
SUPERI*EATES VAFOUR

t Bew Foint
L-tl G'tlfVe, y vs" T

\ VAPOUR.
d' \ LlQutB
6
\- MxruRE
# Euhbte \
TI
E
{J
Poi"i' \
Gurve.
i-" t-
x vs. T ST ECOOLED UeUtD

0.0 1.0

Concentration {mole fraction A, XA or yn)

Fignl.e 7,11 Constant pressure phase diagram

Usually the mole fraction of the more volatile component is ploited on the horizontal axis,
whereby x is the mole fraction in the liquid phase and y is the mole fraction in the
vapour phase,

From the above constant pressure phase diagram; it shows that:

' Since the boiling point of pure A (ta at xa = 1.0) is lower than boiling point of pure
B (ts at Xa = 0.0, i.e. xs = 1.0), therefore component A is more volatile than
component B where A has a lower boiling point than B.

Boiling point and condensation point changes with concentration: Saturated liquid
curve : x vs. T, bubble point curve Saturated vapour curve :y vs. T, dew point
CU TVE

' At each temperature, the vapour and the liquid are in equilibrium

' Three different regions exist where only vapour, only liquid and a vapour-liquid
mixture can exist.

The upper curve in the diagram is called the dew-point curve while the lower one is
called the bubble-point curve. The dew-point is the temperature at which the saturated
vapour starts to condense. The bubble-point is the temperature at which the Iiquid starts
to boil.

The region above the dew-point curve shows the equilibrium composition of the
superheated vapour while the region below the bubble-point curve shows the equilibrium
composition of the subcooled liquid.
ryHHhfl SEPAR.ATION PROCESSES LABORATORY II

For example, when a subcooled liquid with mole fraction of A:0.4 (point
A) is heated, its
concentration remains constant until it reaches the bubble-point (point
B), when rt starts
io boil The vapour evolved during the boiling has the equilibrium composition given
by
point C, approximately 0.8 mole fraction A. This is approximately
50% richer in A than
the original liquid,

Meanwhile, Figure 7.2 below (left) showed an example of typical

equilibrium curve for a
binary mixture on x-y plot. it contains less information than the phase
diagram (i.e,
temperature is not included), but it is most commonly used. It is useful
for graphical
design in determining the number of theoretical stages required
for a distillation column,

EquliLrium Ottre for BBlzerc-TduBE S/*nl at t dm

100

!sD
r;.11]],1 1:,i:;1r;l'' 1,,,1:1:,' r,-l: lli; 1;r-,
! 60

a oto
€

tarr
G

i!t \\
g
o
D30

=
c:0 45o Diagonal Line
D.10

o$
!ot 0.10 ia.2o rl30 OlD 05t a E ri.r-O !.S 0.9 I D,1

ri'ioi: iraCicr 6enz ere i;: rigi:irr. ;r

FiEure 7.2: Constant pressure equiiibrium curve or x_y plot

ffiKITM SEPARATION PROCESSES LABORATORY II

Experimental Result

in this experiment, you need to identify the required data from the experimental work in
order to produce the graph of vapour-liquid equilibrium for the studied system. Then, all
the data must be recorded in a table"

Example of the table of experimental result is as Table 7.1:

Table 7.1: Experimental result of vapour-liquid equilibrium

[Metfilat'no,l !4fater. e.lqn*nd fi-uqufid \{apourr Borffimg

;smase imltiase aftei. 113!tase
r'6
lr3@nrnt
,nefon"e ireeatnmg
,teaEIp'rg
50 200
100 150
t25 725
150 100
200 50

Results and Discussion

Questions

The following questions must be explained explicitly in the result and discussion.

1, Draw the process flow diagram for the entire vapour-liquid equilibrium system.
Explain the process thoroughly.

2. PIot a graph of refractive index versus mol fraction of methanol (before heating).

3. Plot Txy diagram of methanol-water system. Then compare the experimentally

obtained temperature and composition values at equilibrium with the Iiterature
results. Discuss the factors that influence the findings.

4. Describe the uses of VLE diagram.

 SEPARATION PROCESSES LABORATORY
ffi,HHhH II

Table 7.2: Equilibrium data for methanoi-water system

,m. I "z.,uv rn,-o:io rrr:Jtn,arioi:

'72.O 56. s 80.5

7 7.5 58.5 B 1.6

71.4 60.0 83. 1

7 0.6 66.2 otr 7/

o),

69.9 67.5 86.5

69.6 7 0.a 87.4

69. 1 77.4 87, B

67.8 80.0 91. B

66,9 85.0 93.0

66.50 BB, OB 94.I7

66.2 89.0 95,6

oo. l 90.0 96.1

65.7 92,0 96.5

65.4 95.0 98,1

64.95 96.57 95.69

64.7 0 98.71 97.78
64.6 100.0 10 0.0