SEPARATION PROCESS FUNDAMENTALS LABORATORY

EP 316
LABORATORY MANUAL

Lecturer/Instructor: _______________________________

Name

:____________________________

Student ID

:____________________________

Course

:____________________________

FACULTY OF ENGINEERING, TECHNOLOGY &

BUILT ENVIRONMENT
UCSI UNIVERSITY

MAY - AUG 2015

GENERAL INSTRUCTIONS
The experiments in this manual are designed to give engineering

students an introduction to material science including aspects such as

atomic structure, material properties and testing. These experiments are also
intended to teach students the principles of laboratory protocol and
reporting.
Students are required to carry out all the experiments following the
general methods and procedures presented in this manual. All experiments
are to be completed within the allotted time. Students are expected to be
prepared prior to coming for the laboratory session. This includes reading the
lab procedure thoroughly and understanding the objectives, operations and
hazards that may be encountered during the experiment.
The laboratory experiments shall be conducted in groups. Thus,
students have to learn to organize themselves within the groups and to
allocate responsibilities among themselves.

LABORATORY PROCEDURE AND CONTROL

2.1 Logbook
You are required to keep a logbook for experiments. This must be a bound
logbook. You are required to translate the procedure of each experiment in
the laboratory manual into graphical illustrations or a flowchart in your
logbook before you start.
Record in your logbook every action and observation as you carry out the
experiment. Records should be as brief, but concise, as possible.

Each experiment in the logbook should contain the following information:

(i) Title of the experiment

(ii) Date of the experiment carried out
(iii) Objective of the experiment
(iv) Hypothesis of the experiment
(v) Procedure outline or brief description of the method
(vi) Observation (should be recorded throughout the experiment)
A logbook should be neat. Clarity of procedure and results are
important. Always use a pen to write on your logbook. Mistakes made should
be crossed out clearly. Use of liquid paper or eraser is not allowed.
The lab instructor/lecturer will inspect and sign your logbook during the
lab session and possibly grade them at the end of the semester.
2.2 Laboratory group
You will be assigned into a group (please refer to the student notice
board or outside the lab after the first session of the laboratory meet up).
Students are not allowed to change groups. You are required to work with
your group members as much as possible in terms of understanding the
experiment and sharing information on the different activities performed by
different members. At the end of each of the session, each of the group
members is required to carry out peer evaluation. Peer evaluation is private
and confidential. The purpose of peer evaluation is to ensure that all group
members contribute throughout the laboratory session.

2.3 Laboratory Reports

Each student will be responsible for preparing an individual report after

completing each laboratory experiment.
(a)

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

(b)

Report style/format
Reports may be hand-written or typed-written. If typed-written, text

shall be
spaced, using font type New Times Roman and font size 12. It is
recommended that an equation editor be used, otherwise, equations
may be handwritten. Atomic structures and other figures may be
drawn by hand.
The report shall be:
(i)

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

was weighed.

(ii)

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

(iii)

(c)

Plagiarism will not be tolerated.

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

Front page (Refer to Appendix A)

(ii)

Table of contents (Refer to Appendix B)

(iii)

Introduction/background of the experiment

Contains a summary of the experiment that is carried out. This

section
includes

the

statement

of

purpose

or

objectives

of

the

experiment and an introduction to the technique used. It is not

necessary to include a discussion of the basic theory relevant to
the experiment. The introduction of the report should not be
more than 20% of the overall report.
(iv)

Material and Methodology

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

(v)

Results and discussion

Test results obtained from the experiment shall be presented in
the

applicable

format:

Narrative,

tabular,

graphical,

photographic, or a combination of the above. Numerical data

must be presented realistically with appropriate number of
decimal places. Data should be tabulated neatly showing raw
experimental data, if necessary, and reduced (useful) data.
Calculations for reduced data should be briefly described and
need not be worked out. Identify formulas, charts, tables or
handbooks that were used to obtain the final result. If needed,
you may refer sample calculations to the appendix. Any
questions given in the lab sheet should be answered in the
Discussion section.
(vi)

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

(vii)

Limitation of the Experiment/Difficulties Encountered (if any)

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

(viii)

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

(ix)

Appendix (if any)

Laboratory Safety
All safety requirements as specified in this section will be strictly
enforced. Students are required to comply with the following rules when in
the lab.
1.

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

2.

Wear suitable attire for lab work. Do not wear loose or bulky clothes,

ties or
jewelery when working around rotating equipment. Students with long
hair must tie their hair before entering the lab. Open-toe shoes and
sandals are not permitted. (Lecturer/instructor reserves the right not to allow
students who do not follow this rule to enter the lab).
3.

Eating and drinking in the lab are strictly prohibited.

4.

All hand phones must be switched off.

5.

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

perform the experiment.

6.

Students must have a towel (for cleaning purposes), a logbook and

their lab manual during the lab session.

7.

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

start of the lab.

8.

Clean the bench and return all apparatus to their respective places
before you leave the lab.

9.

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

10.

Dispose of excess reagents as instructed, never return excess reagents

into the bottle. Some used chemicals may be washed down the drain,
while others require a different method of disposal. If a chemical can
go in the sink, be sure to wash it away thoroughly rather than risk an
unexpected reaction between chemical leftovers later.

11.

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

12.

Handle all equipment with care to avoid damage during experimental

operations.

13.

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

immediately.

EXPERIMENT 1: SIEVE TEST ANALYSIS

OBJECTIVE
1. To determine the particle size distribution by sieving technique
THEORY
Sieving is one of the few principal methods, in which a relatively large quantity of material is
physically subdivided in size classes. The separated fractions can be accurately weighed and,
thus, the determination of the size distribution functionbased on massmay be accurate. The
major advantages of the sieving technique are that it allows relatively large samples for analysis
or separation, that the principles are easy to understand and that the sieves and sieving equipment
are relatively cheap. Also, size fractions are being obtained, which can be used for other purposes
(e.g., further analysis or product testing).
APPARATUS
Sieve shaker, electric balance, spanner, brush, soil/sand.

PROCEDURE
1. Clean each sieve and the bottom pan using the provided brush. Weigh the sieve and the
bottom pan individually and record the data.
2. Weigh 1kg of sample (soil/sand).
3. Arrange the sieve with biggest aperture size at the top and lowest at the bottom and
finally the pan at the most bottom.
4. Shake the stack for a specified length of time at a preset speed.
5. When shaking is complete, weigh each sieve again individually.
6. Record the weight of sample retained from each sieve and the pan.
7. Complete the table given.
RESULTS AND DISCUSSION
# of Aperture
sieve
size
(mm)

Mass of
empty
sieve

Mass of
sieve + retain
sample

Sieve fraction

1
2
3
4
5
6
7
Pan
Total

Cumulative
retained
%

Cumulative
undersize
%

Cumulative undersize = 100 Cumulative retained

Original mass

wt =

Total of fraction masses

w1 =

Loss

wt w1
x100%
wt

=____________% (ok if less than 2%)

In your discussion, you should include the following:
1. Plot the graph of cumulative undersize against average particle size.
2. Determine the particle size at % cumulative 16%, 50%, and 84%
3. Calculate the particle size distribution using formula:
Size distribution

p84 p16
2

4. Discuss why sieving process is important in chemical engineering.

CONCLUSION
State the conclusion of the experiment.
REFERENCE:
1. Mc Cabe, W.L, Smith, J.C. & Harriot, P., Unit Operation of Chemical Engineering, 4th
Edition, Mc Graw-Hill, 1985.

EXPERIMENT 2: BATCH SEDIMENTATION TEST

OBJECTIVE
1. Learning the fundamental principle of separation of solids from suspensions
2. To determine the rate of sedimentation of a sample of particles in a liquid
3. To plot a graph between the suspension density at a certain vertical position against time
THEORY
Sedimentation uses gravitational forces to separate particulate material from fluid streams. The
particles are usually solid, but they can be small liquid droplets, and the fluid can be either a
liquid or a gas. In sedimentation, particles are falling from rest under the force of gravity.
Therefore in sedimentation, takes the familiar form of Stokes' Law:
UT = x2g(p - f)/18
where p = density of particle, kg m-3
f = density of fluid, kg m-3
g = gravity, m s-2
x=
particle diameter, m
=
molecular viscosity, N s m-2
UT = terminal settling velocity, m s-1
Stokes Law applies only in streamline flow and strictly only to spherical particles. Stokes
solution is applicable for settling at low Reynolds numbers (Re<< 1). Stokes Law applies only to
cases in which settling is free, that is where the motion of one particle is unaffected by the
motion of other particles. The objective of sedimentation process analysis is to determine the rate
at which solid particles accumulate in the lower end of the container. A graph of the interface
height versus time is known as the sedimentation curve.

MATERIAL AND APPARATUS

Graduated cylinder, stop watch, ruler, stirring rod, beaker, chalk and water.
Pre-lab assignment:
The force balance for a settling particle (at terminal velocity) is Fdrag = M g- Fbuoyancy
(where g is the gravitational acceleration, Fdrag is drag force, M is the particles mass and Fbuoyancy
is buoyancy force, V f g, V is the particles volume )
And thus, Fdrag = (p - f ) g D3 /6
Fdrag = 3 f D UT
Derive Stokess Law.
PROCEDURE
1. Prepare a 500mL graduated cylinder with a ruler.
2. Weigh 10g of sample and put in a beaker. Fill in the beaker with 300-400mL of tap water.
Mix suspension vigorously to achieve even mixing. Transfer the suspension to the
prepared graduated cylinder.
3. The start-time for measurement is when the object has reached several centimeters below
the surface and stop-time is several centimeters above bottom.
4. For every five seconds interval, record the height of the clear area.
5. Repeat the same process for 3 times and the average height was recorded.
6. Plot the graph of the interface height versus time. From the graph, calculate the settling
velocity of suspension at any point of time. Then, determine the particle diameter, x.
7. Discuss the graph that you have plotted.

RESULTS AND DISCUSSION

Time

Height

Given Question:
Calculate the settling velocity of dust particles of
(a) 60mm and
(b) 10mm diameter
in air at 21C and 100kPa pressure. Assume that the particles are spherical and of density 1280
kg m-3, and that the viscosity of air = 1.8 x 1-5 N s m-2 and density of air = 1.2 kg m-3.
CONCLUSION
State the conclusion of the experiment.
REFERENCE
State the reference used.

EXPERIMENT 3: CENTRIFUGATION
OBJECTIVES
1. Recognize the fundamentals of centrifugation
2. Operate a centrifuge at a pilot scale

INTRODUCTION
The centrifuge is a widely used instrument for the separation of components. This operation is a
separation process that uses centrifugal force to separate two mixed liquids or insoluble solids
from liquids (suspension). The centrifuge works using the sedimentation principle, where the
centripetal acceleration causes more dense substances to separate out along the radial direction
(the bottom of the tube). By the same token, lighter objects will tend to move to the top (of the
tube; in the rotating picture, move to the centre).
THEORY
Protocols for centrifugation typically specify the amount of acceleration to be applied to the
sample, rather than specifying a rotational speed such as revolutions per minute. The acceleration
is often quoted in multiples of g, the standard acceleration due to gravity at the Earth's surface.
This distinction is important because two rotors with different diameters running at the same
rotational speed will subject samples to different accelerations. Since the motion is circular the
acceleration can be calculated as the product of the radius and the square of the angular velocity.
Traditionally named "Relative centrifugal force" (RCF), it is the measurement of the acceleration
applied to a sample within a centrifuge and it is measured in units of gravity (times gravity or
"g"). It is given by

where
is earth's gravitational acceleration,
is the rotational radius,
is the rotating speed, measured in revolutions per unit of time.
When the rotational speed is given in revolutions per minute (RPM) and the rotational radius is
expressed in centimeters (cm) the above relationship becomes :

is the rotational radius measured in centimeters (cm),

is rotating speed measured in revolutions per minute (RPM).
MATERIAL AND APPARATUS
Centrifuge unit, centrifuge tube, ruler, sample (ferrocene + toluene/sugar cane /chocolate drink)

PROCEDURE
1. Ensure an authorized member of staff outside the laboratory is made aware that the
centrifuge is going to be operated with the information provided on the test procedure
sheet. This person should be notified again once the test is complete.
2. Turn on the main power ON using the switch on left hand side of the centrifuge.
3. The LED displays will indicate the current status and settings.
4. Press the LID key to unlatch the lid.
5. Insert an appropriate adaptor for the glassware to be used into each of the four buckets.
6. Insert the glassware, loaded with sample, into the adaptors,
CAUTION: TWO OR FOUR SAMPLES CAN BE CENTRIFUGED AT THE SAME TIME,
CENTRIFUGING ONE OR THREE SAMPLES WILL CAUSE AN IMBALANCE OF THE
ROTOR AND MAY RESULT IN DAMAGE TO THE CENTRIFUGE.
IF ONLY TWO SAMPLES ARE BEING CENTRIFUGED, THE GLASSWARE
CONTAINING THE SAMPLES MUST BE PLACED OPPOSITE EACH OTHER IN THE
ROTOR.
7. Check tightness of rotor nut before operation.
WARNING: THE MAXIMUM LOADING OF THE ROTOR AND THE MAXIMUM
PERMISABLE REVOLUTIONS PER MINUTE MUST NOT BE EXCEEDED (SEE
LABEL ON ROTOR).
8. Push the lid closed and hold it until the latch is felt to start to pull the lid down onto the
seal.
9. Press the SPEED/RCF key to toggle between speed (in rpm) and Relative Centrifugal
Force (in g).
10. Rotate the Time Control until the required value is shown on the Timer display.
11. The temperature to be set is entered into the Set Temperature display by rotating the
Temperature control.
12. Press the START key to commence a run.
RESULT AND DISCUSSION
What would be the expected result if a different centrifugation speed has been selected?
CONCLUSION

State your conclusion.

REFERENCE
State the reference used.

EXPERIMENT 4: SEPARATION OF SOLID MIXTURE

Mixtures are not unique to chemistry, we use and consume them on a daily basis. The beverages
we drink each morning, the fuel we use in our automobiles, and the ground we walk on are
mixtures. Very few materials we encounter are pure. Any material made up of two or more
substances that are not chemically combined is a mixture.
The isolation of pure components of a mixture requires the separation of one component from
another. Chemist have developed techniques for doing this. These methods take advantage of the

differences in physical properties of the component. The technique to be demonstrated in this

laboratory are the following:
Extraction: this uses a solvent to selectively dissolve one component of the solid mixture.
With this technique, a soluble solid can be separated from an insoluble solid.
Decantation: This separates a liquid from insoluble solid sediment by carefully pouring
the liquid from the solid without disturbing the solid.
Recrystallization :This involves dissolving a mixture of solids in a hot solvent, followed
by cooling, and crystallization of the more insoluble material.
Filtration : This separates a solid from a liquid through the use of a porous material as a
filter. Paper, charcoal, or sand can serve as filter. These materials allow the liquid to pass
through but not the solid.
Objective :

Separate the substances.

Determine the percent of each in the original mixture.

Materials and apparatus:

Sand, benzoic acid, tap water, sodium chloride

Beaker, hot plate, filter funnel, stirring rod.

Result and Calculation:

1. Calculate the percent of each component in the mixture. Show your calculation.
2. Calculate the percent error in your result. Show your calculation.
EXPERIMENT 5: DRAG COEFFICIENT MEASUREMENT
Objective:

To analyze the phenomena of free-falling body in any fluid.

To Determine the following parameters:

1) Terminal velocity
2) Drag coefficient vs Reynolds number

3) Fluid viscosity
4) Sphere diameter
Introduction.
Any solid object moving through a viscous fluid will experience a resistance or drag force. This
is one of the most important aspects of fluid mechanics and it must be remembered that common
fluids like air and water must be considered viscous in this context. An understanding of fluid
drag forces is therefore essential to the proper design of aircraft, trains, automobiles, ships,
submarines, tall structures, jetties and off-shore structures of all kinds. It is equally relevant to
the mechanics of particles falling under gravity; raindrops and parachutes in air, sand grain in air
or water and the settlement of kinds of all suspended solid particles in water. The drag force
depends on a number of variables and one of the more important is the shape of the moving
body. In this experiment only spherical objects are used. This enables the relationships between
more easily described parameters such as velocity, fluid viscosity and body density to be
explored experimentally. For spherical objects the radius is a sufficient description of the object
although the specific weight of each material used must be determined as well.
Result and Calculation.
1. Discuss whether the liquids used are Newtonian or Non-Newtonian.
2. What is the relationship between CD and Reynolds number?
3. Plot CD and Re values obtained experimentally on a log-log graph. Comment on the
agreement between the experimental points and the Stokes line.