Department of Chemical Engineering

Unit Operation Lab

ChE-422 Manual

Instructors:

Dr. Karim Kriaa

Eng. Najem Alarwan

STUDENT NAME:

STUDENT NUMBER:

SEMESTER / YEAR:
 EXPERIMENT #01 (UO-01)

MOLECULAR DIFFUSION IN GASES

OBJECTIVE:

To determine the diffusion coefficient

THEORITICAL BACKGROUND

Molecular diffusion or molecular transport can be defined as the transfer or movement of

individual molecules through a fluid by means of the random, individual movements of the
molecules.

The diffusivity of the vapor of a volatile liquid in air can be determined by winklemann’s
method in which liquid is contained in a narrow diameter vertical tube, maintained at a
constant temperature. A stream is passed over the top of the tube to ensure that the partial
pressure of the vapor is transferred from the surface of the liquid to the air stream by
molecular diffusion. With this method, the diffusion is the same as gas A diffusing in stagnant,
nondiffusing B.
𝐶 𝐶
𝑁𝐴 = 𝐷 ( 𝐿𝐴 ) (𝐶 𝑇 ) (2.1)
𝐵𝑚

The evaporation of the liquid A is expressed as follows

ρL dL
NA = (2.2)
M dt

Equating the above equations, integrating and rearranging the resulting equation, one can
obtain as follows:
t L ρ C ρ C
(L−L0 )
= (2MD ) (C Bm L Bm
) (L − L0 ) + (MDC ) L0 (2.3)
C A T C A T

𝑡
The above equation is indeed a linear correlation between (𝐿−𝐿 ) against (𝐿 − 𝐿0 ) with slope =
0
𝜌𝐿 𝐶𝐵𝑚
(2𝑀𝐷 ) (𝐶 )
𝐴 𝐶𝑇

𝑡
Thus by plotting (𝐿−𝐿0 )
versus (𝐿 − 𝐿0 ), one can easily calculate the slope and find the
diffusivity coefficient of gas A in B.
1 𝑇𝐴𝑏𝑠
𝐶𝑇 = 22.414 ( ) (2.4)
𝑇𝑎

(𝐶𝐵1 −𝐶𝐵2 )
𝐶𝐵𝑚 = 𝐶 (2.5)
𝑙𝑛( 𝐵1 )
𝐶𝐵2

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𝐶𝐵1 = 𝐶𝑇 (2.6)
𝑃𝑎 −𝑃𝑉
𝐶𝐵2 = ( ) 𝐶𝑇 (2.7)
𝑃𝑎

𝑃
𝐶𝐴 = ( 𝑃𝑉 ) 𝐶𝑇 (2.8)
𝑎

DESCRIPTION OF THE EQUIPMENT

Figure 2.1. Linear Conduction Heat Transfer Unit

The liquid that is to be volatilized is placed in capillary tube. The capillary tube is placed inside
a water bath whose temperature is carefully controlled by a controller. The height of the liquid
that decreases by time is observed using microscope equipped with Vernier height gauge.

EXPERIMENTAL PROCEDURE

1. Fill the capillary tube with acetone to a depth of approximately 35 mm.

2. Insert capillary tube through a rubber ring, inside the metal nut until the top of tube rest on
the top of the nut.

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3. Screw gently the above assembly onto the top plate, with the ‘T’ piece normal to the
microscope
4. Connect flexible air tube to one end of the ‘T’ piece.
5. Set up the microscope as shown in figure 4.1. and adjust the object lens to within 20-30 mm
from the tank.
6. Adjust the vertical height of the microscope until the capillary tube is visible (if the capillary
tube is still not visible adjust the distance from the object lens to the tank until it is visible).
7. Adjust viewing microscope until the meniscus inside the capillary tube clear and well
defined (note that the image in the microscope is upside down. That means the top of the
image is the bottom of the capillary tube).
8. Make sure that the sliding Vernier scale should be aligned with a suitable graduation on the
fixed scale.
9. Switch on the air pump.
10. Adjust the air flow rate using the Hoffman clip on the flexible tube so the flow rate is low.
11. Record the level inside the capillary tube.
12. Switch on the temperature controlled water bath and adjust set point on controller to 40 oC
to obtain steady temperature at 40 oC.
13. Switch off the temperature controlled water bath after approximately 60 minutes to
prevent air bubbles.
14. Record the change in level inside the capillary tube.
15. Repeat #12 - #14.

REFERENCES

Geankoplis,C.J., “Separation Processes and Unit Operations, 4th edition, Prentice-Hall Inc., New
Jersey, 2004

”CERa Experiment Instruction”, armfield, 2011.

NOTATION

CA : Saturation concentration of acetone at interface, kmol/m3

CBm : Logarithmic mean molecular concentration of vapor, kmol/m3
CT : Total concentration, kmol/m3
D : Diffusivity coefficient, m2/s
L : Effective distance of mass transfer (m)
M : Molecular weight of acetone, kg/mol
NA : Molar flux, mol/m2.sec
Pa : Atmospheric pressure, atm
PV : Vapor pressure of acetone, atm
L : Density of acetone, kg/m3
T : Time, sec
Ta : Bath temperature, K
Tabs : Absolute temperature, K

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 WORK SHEET

Time, ks Liquid level 𝑡

(L-L0) (𝐿 − 𝐿 0 )

Do the following:
𝑡
1. Plot between (𝐿−𝐿 ) and (𝐿 − 𝐿0 )
0
2. Calculate diffusivity coefficient from the slope of the line.
3. Compare your findings with theoretical value. (refer to mass transfer course)

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 EXPERIMENT #02 (UO-02)
CONVECTION DRYING
OBJECTIVE:

1. To determine the reduction in weight and the drying rate over time during the drying
process.
2. To investigate the effect of air flow rate in convection drying.

THEORITICAL BACKGROUND

Drying is a physical process of removing the liquid adhering to a material and contained within
it. In drying process, the water is usually removed as a vapor by air. It proceeds more slowly for
the moisture that is located in capillaries and pores within the material to be dried. This is
because the capillary forces or diffusion resistance must be overcome. The removal of water of
crystallization contained in the material to be dried is even more difficult because it is bounded
by relatively strong molecular forces. The material must be intensely heated to expel the water.

According to the type of heat transfer, drying process can also be classified as follows:

1. Convection drying when the heat for the drying is transferred to the material to be dried
by a flowing gas.
2. Contact drying when the heat is transferred from the heater to the material by
conduction due to physical contact between them.
3. Radiation drying when the heat is transferred by radiation. The source of energy can be
in form of electromagnetic radiation, infrared, microwave or even radio frequency.

In many cases, drying is carried out using warm air at atmospheric pressure. This drying process
is called air drying. If drying is done at significant sub atmospheric pressure, it is called vacuum
drying. In some cases, the moisture in the material is cooled and frozen and using convection,
conduction or radiation heat transfer, and the freezing moisture can be sublimed. This method
of drying is known as freezing drying.

One of the most important analyses in drying is rate of drying curves. The equilibrium moisture
contents of various materials cannot be predicted and must be determined experimentally.
Similarly, since the basic mechanism of rates of drying is quite incomplete thus it is necessary in
most cases to obtain some experimental measurements of drying rates.

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DESCRIPTION OF THE EQUIPMENT

1. Drying channel 2. Drying plates 3. Transparent door

4. Process schematic 5. Air velocity sensor 6. Measuring point for
humidity and temperature
7. Digital balance 8. Bracket for fying 9. Measuring point with
plates humidity and temperature
sensor
10. Switch cabinet with 11. Fan
digital displays

EXPERIMENTAL PROCEDURE

1. Remove drying plates from support frame.

2. Tare scale to zero
3. Insert drying plates individually into support frame, read off and note the weight of the
individual drying plates on the digital scale.
4. Switch on fan and set speed using flow rate gauge e.g. 1.3 m/s.
5. Read off volumetric air flow from display and make a note of it.
6. Switch on heater and set the temperature controller e.g. 50oC.
7. Run air conditioning duct until it is warmed up evenly all along its length.
8. Spread material (gravel with grain size of 0.5-0.7 mm) to be dried in a thin layer on the
drying plates.
9. Insert drying plates in the support frame and note the total weight.
10. Tare scale to zero.

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11. Introduce water to the spread material e.g. 50 g
12. Start drying experiment, commence time measurement using stopwatch.
13. Record air temperature T2 after material to be dried, relative humidity after material being
dried, total mass m of material to be dried (material and drying plates).
14. Stop the experiment when the mass m of material to be dried does not change significantly.
15. Repeat the experiment for air speed of 2 m/s.

REFERENCES

Transport Processes and Separation Process Principles, 4th ed., 2003, C.J. Geankoplis, Pearson
Education, Inc.

CE 130 GUNT Experiment Manual.

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 WORK SHEETS

Experiment #1
Mass of drying plate 1 :
Mass of drying plate 2 :
Mass of drying plate 3 :
Dry Gravel mass :
Introduced water :
Total Mass :
Air speed :
Heating level :

Time T1 1 T2 2 WT
o o
min C % R.H. C % R.H. g
Before plate After plate

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Experiment #2
Mass of drying plate 1 :
Mass of drying plate 2 :
Mass of drying plate 3 :
Dry Gravel mass :
Introduced water :
Total Mass :
Air speed :
Heating level :
Time T1 1 T2 2 WT
o o
min C % R.H. C % R.H. g
Before plate After plate

1. Plot the moisture content versus time for both experiments, comment on it in the discussion
part.
2. Plot the drying rate versus time for both experiments, determine which part is constant drying
rate period and which part is falling rate period. comment on it in the discussion part.
3. Find the graphical value of constant drying rate.
4. predict value of constant drying rate.
5. Compare the value from #3 and #4. Comment on the result.

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 EXPERIMENT #03 (UO-03)
WET COOLING TOWER
OBJECTIVE:

To investigate and understand the influence of volumetric air flow rate, volumetric water flow
rate and packing density on the performance parameters of the cooling tower.

THEORITICAL BACKGROUND

Water or wet cooling tower is one of the most important types of process in the process
industries. This type of cooling tower follows the principle of evaporative cooling. There are
many cases in industry in which warm water is discharged from heat exchangers and
condensers when it would be more economical to cool and reuse it than to discard it.

In a typical water-cooling tower, warm water flows counter currently to an air stream. Typically,
the warm water enters the top of a packed tower and cascades down through the packing,
leaving at the bottom. Air enters at the bottom of the tower and flows upward through the
descending water. The tower packing often consists of slats of plastic or packed bed. The water
is distributed by troughs and overflows to cascade over slat gratings or packing that provides
large interfacial areas of contact between the water and air in the form of droplets and films of
water.

In this cooling tower, water evaporates into air because its vapor pressure in the air is less than
the saturation vapor pressure. The amount of heat that is needed to evaporate the liquid is
drawn from the air. Furthermore, this air cools water in contact with it. In this case, the wet-
bulb temperature which takes both temperature and humidity into account, as compared to
the actual air temperature (dry-bulb temperature), is a measure of the potential for
evaporative cooling. The greater the difference between the two temperatures, the greater the
evaporative cooling effect. Therefore, wet-bulb temperature is essentially the lowest
temperature which can be attained by evaporative cooling at a given temperature and
humidity.

Several characteristic variables are calculated as follows

Cooling range which is the difference between the warm water temperature at the inlet to the
cooling tower and the cold water temperature at the outlet from the cooling tower

𝑧 = 𝑇4 − 𝑇5 (1.1)

Wet bulb approach which is the difference between the cold water temperature at the cooling
tower outlet and the cooling limit or wet bulb temperature.

𝑎 = 𝑇5 − 𝑇𝑓1 (1.2)

Cooling coefficient is formulated as follows

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 𝑇 −𝑇
𝜂 = 𝑇 4−𝑇 5 (1.3)
4 𝑓1

Water loss due open circuit in cooling tower is calculated as follows

𝑚̇𝑊 = (𝑋2 − 𝑋1 )𝑚̇𝐿 (1.4)

Heat load which is the heat which is taken from the water during the cooling process is
formulated

𝑄̇𝑊 = 𝑚̇𝑊 𝐶𝑝𝑊 𝑧 (1.5)

Actual air mass flow rate is calculated as follows:

(𝑃1−𝑃2)
𝑚̇𝐿 = 𝛼𝜀𝑐√ (1.6)
𝑣2

 = 0.605;  = 0.98, c = 0.0073 and the volumetric air flow is calculated

𝑉𝐿̇ = 𝑚̇𝐿 𝑣2 (1.7)

Cooling capacity which is the difference in enthalpy between the air inlet and outlet

𝑄̇𝐿 = (ℎ2 − ℎ1 )𝑚̇𝐿 (1.8)

DESCRIPTION OF THE EQUIPMENT

Figure 1.1 Wet Cooling Tower

The main wet cooling tower unit can be seen in figure 1. The water is heated using heating
element in a tank (7), pumped (6) and then sprayed from the top of the column through nozzle
(1) and intimately contact with cooling air due to the packing (2). The air comes in from the air
chamber (4) at the bottom of the column. The air flow rate is adjustable using fan (5). Due to

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evaporation during the course of the process, the make-up water (8) is required to maintain
enough water for the process. All parameter readings including water and air flow rate as well
as temperature can be collected manually from the display and control buttons (3). The column
is also equipped with temperature/humidity sensor (9) at the top and the bottom.

EXPERIMENTAL PROCEDURE

Prior to experiment, it is important to do the following steps:

Experiment #1: investigation on the effect of water flow rate.

1. Fill the water tank and the supply tank (make-up water tank)
2. Choose the packing type 1 and assemble it.
3. Connect all sensors (combined temperature/humidity and temperature sensors)
4. Connect the system to the mains electricity supply.
5. Turn on the heater and select the heating level 2 i.e. 1 kW and heat the water in the
tank up to 40 oC.
6. Turn on the fan and adjust the air flow rate so the pressure difference is approximately
120 Pa by changing the shutter opening.
7. Turn on the pump and adjust the volumetric water flow rate at 60 L/h.
8. After reaching steady state (app. 20 mins), take all measurement readings from the
display and fill out worksheet.
9. Repeat the same procedure for water flow rate of 75 L/h and 90 L/h.

Experiment #2: investigation on the effect of air flow rate.

1. Reduce the speed down to 60 L/h.

2. After reaching steady state (app. 10 mins), take all measurement readings.
3. Repeat the same procedure for p of 140 pa and 160 Pa.

Experiment #3: investigation on the effect of packing density.

1. Turn off the heater, fan and pump. Disconnect all sensors and replace the packing type
with type #4.
2. Connect all sensors (combined temperature/humidity and temperature sensors)
3. Connect the system to the mains electricity supply.
4. Turn on the heater and select the heating level 2 i.e. 1 kW and heat the water in the
tank up to 40 oC.
5. Turn on the fan and adjust the air flow rate so the pressure difference is approximately
120 Pa by changing the shutter opening.
6. Turn on the pump and adjust the volumetric water flow rate at 60 L/h.
7. After reaching steady state (app. 20 mins), take all measurement readings from the
display and fill out worksheet.

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REFERENCES

Geankoplis,C.J., “Separation Processes and Unit Operations, 4th edition, Prentice-Hall Inc., New
Jersey, 2004

Jebavy,F. ,”WL 320 Experiment Instruction”, GUNT, 2007.

NOTATION

a : Wet bulb approach, K

c : Constant, m2
CpW : Specific heat capacity of water, kJ/kg.K
h1 : Enthalphy of outlet air, kJ/kg
h2 : Enthalphy of inlet air, kJ/kg
mL : Air mass flow rate, kg/s
mW : Water mass flow rate, kg/s
P1 : Inlet pressure, Pa
P2 : Outlet pressure, Pa
QW : Heat load, W
T4 : Inlet water temperature, K
T5 : Outlet water temperature, K
Tf1 : Wet bulb temperature, K
VL : Air volumetric flow rate, l/s
X1 : Absolute humidity at outlet air, g/kg
X2 : Absolute humidity at inlet air, g/kg
z : Cooling range, K
 : Flow Coefficient
 : Expansion Coefficient
 : Cooling Coefficient
2 : Kinematic Viscocity, m3/kg

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 WORK SHEETS

Experiment #1

Parameter Run 1 Run 2 Run 3

AB, m2/m3 110 110 110
T1, oC
 1, %
T2, oC
 2, %
T4, oC
T5, oC
P, Pa 120 120 120
Fw, l/min 60 75 90

Experiment #2

Parameter Run 1 Run 2

AB, m2/m3 110 110
T1, oC
 1, %
T2, oC
 2, %
T4, oC
T5, oC
P, Pa 140 160
Fw, l/min 60 60

Experiment #3

Parameter Run 1
AB, m2/m3 200
T1, oC
 1, %
T2, oC
 2, %
T4, oC
T5, oC
P, Pa 120
Fw, l/min 60

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 .EXPERIMENT #04 (UO-04)
FLUIDIZED BED
OBJECTIVE:

1. To investigate the loosening speed of a fluidized bed in air and water medium.
2. To determine the relationship between flow rate and the depth of the fluidized bed.
3. To investigate the effect of particle size on fluidization.

THEORITICAL BACKGROUND

Fluidized beds are widely used in process technology. One of important applications in chemical
technology is fluidized bed reactor in which variety of multiphase chemical reactions is carried
out. In a fluidized bed, a layer of fine granular solid matter is loosened by a fluid flowing
through it to such extent that the particles of solid matter are free to move within certain
limits. The layer of solid material takes on similar properties to a fluid.

To characterize a fluidized bed, the pressure loss of the fluid flowing through the bed can be
used. When a fluid flows through the mass initially the pressure underneath the mass increases
as the flow speed increases until the pressure forces match the weight of the mass, and the
mass becomes suspended. With further increasing flow rate, the layer set in motion and
reaches a fluidized state. At this condition the static solid-like state changes to dynamic-like
state. The pressure loss now remains almost constant even with further increasing flow rate.
From a certain flow rate the particles at the top no longer fall back into the fluidized bed, they
are drawn off by the fluid flow and removed.

Pressure losses in fluidized bed can be calculated as follows:

𝜌
∆𝑝 = 𝑔 (1 − 𝜌𝑓 ) ℎ𝜌𝑝𝑠 (3.1)
𝑝

Meanwhile loosening speed at which the mass of solid matter passes the transition to a
fluidized bed is expressed
𝑅𝑒𝑙𝑜
𝑤𝑙𝑜 = 𝑣𝑓 (3.2)
𝑑𝑝

For irregular shape, loosening speed must be corrected,

𝑤 = 𝑤𝑙𝑜 𝜑 (3.3)

The void fraction of a bed is expressed

𝜌𝑝𝑠
𝜀 =1− (3.4)
𝜌𝑝

Reynolds’ number is formulated as follows

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 𝜀3
𝑅𝑒𝑙𝑜 = 42.86(1 − 𝜀 ) (√1 + 3.11 × 10−4 𝐴𝑟 (1−𝜀)2 − 1) (3.5)

With Archimedes’ number is defined as follows

3 𝜌 −𝜌
𝑔𝑑𝑝 𝑝 𝑓
𝐴𝑟 = (3.6)
𝜇2 𝜌𝑓

1. water overflow 2. test tank for water 3. 2-tube manometer 4. flow meter for water 5. U-tube
manometer 6. flow meter for air 7. test tank for air 8. filter

EXPERIMENTAL PROCEDURE

Filling, emptying, and cleaning the single tube manometer, 2 tube manometer, and vessel with
particles, including the calibration and testing of vessel for both water and air must be done by
the trained person.

A. Calibration with empty test tank for water and air

1. Connect the pressure measuring connections to the manometer. On a two tube
manometer, the display value can be set to the center of the manometer.
2. Fully open the by pass valve below the rotameter
3. Fully close the needle valve on the rotameter.
4. Turn on the pump

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 5. Increase the flow in small increments by opening the needle valve
6. Continuously note the flow rate and differential pressure in the table.
7. Continue the measurements up to the maximum flow.

B. Experiment with test tank for water

1. Record the initial bed height (h=100 mm) and ensure particle with dp of 0.505 mm is
used.
2. Fully open the bypass valve below the rotameter.
3. Fully close the needle valve on the rotameter.
4. Turn on the pump.
5. Increase the flow in small increments by opening the needle valve.
6. Observe the particle movement, note the flow rate, bed depth, and pressure drop.
7. Continue increase the flow rate until flow rate of 1.5 L/min is obtained (above certain
flow rate, the needle valve will be already fully open, further increase of flow rate must
be done by closing the bypass valve).

C. Experiment with test tank for air

1. Fill the test vessel with particle i.e. dp = 0.240 mm, until the height of the bed is 50 mm.
2. Fully open the by pass valve below the rotameter.
3. Fully close the needle valve on the rotameter.
4. Turn on the compressor.
5. Increase the flow in small increments by opening the needle valve and observe the
mass.
6. Continuously take note of the flow rate and differential pressure.
7. Take the note as soon as the first signs of the particle movements.
8. Continue until the a flow 30 L/min is achieved (above certain flow rate the needle valve
will be already fully open, further increase of flow rate must be done by closing the
bypass valve)
9. Repeat the same procedure for different particle size, i.e. d p=0.505 mm.

REFERENCES

”CE220 Experiment Instruction”, GUNT, 2011.

NOTATION

P : Pressure drop, mm
G : Gravitational acceleration, m/s2
f : Fluid density, kg/m3
p : Particle density, kg/m3
H : Height of mass
ps : Particle mass density, kg/m3
wlo : Fluid velocity between spherical particles, m/s
Relo : Reynolds’ number
dp : Particle diameter, m

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vf : Kinematic viscocity
W : Corrected fluid velocity, m/s
 : Form factor
 : Void fraction
Ar : Archimedes’ number
 : viscocity

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 WORK SHEET

A. Calibration with empty test vessel for water and air.

For water For Air
Q, L/min P,mm W, m/s Q, L/min P,mm W, m/s

B. Experiment with test vessel for water.

Dp = mm
Q, L/min P,mm H, mm W, m/s

















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C. Experiment with test vessel for air.

Dp = mm

Q, L/min P,mm W, m/s

















Dp = mm

Q, L/min P,mm W, m/s

















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Do the following:
1. Plot pressure drop against fluid speed for all data.
2. Plot bed depth against flow rate for test vessel with water only.
3. Determine the loosening velocity (Wlo) for experiment B and C from the plot.
4. Determine the loosening velocity (Wlo) using equation and compare with that
obtained from the plot.
5. Comment on the all above plots.

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 EXPERIMENT #06 (UO-06)
SOLID LIQUID EXTRACTION
OBJECTIVE:

1. To study the performance of discontinuous solid-liquid extraction process.

2. To study the influence of number of stages on counter-flow solid-liquid extraction process.
3. To study the effect of solvent temperature on the extraction performance.

THEORITICAL BACKGROUND

Many biological, inorganic, and organic substances occur in a mixture of different components
in solid. Solid-liquid extraction is general term used for a process to separate either desired or
undesired solute from the solid phase using a solvent/liquid. It is sometimes called leaching and
if it is intended to remove undesirable component from solid using water, it is called washing.

In general the process of solid-liquid extraction can be described as follows; the solvent must be
transferred from the bulk solvent solution to the surface of the solid. The solvent then must
penetrate or diffuse into the solid and the solute dissolves into the solvent. The solute then
diffuses through the solid solvent mixture to the surface of the particle. Finally, the solute is
transferred to the bulk solution.

There are several factors influencing extraction performance for example:

1. Differences in concentration; the greater the difference in concentration of the usable

substance in the extraction material and in the solvent, the greater the driving force when
extracting.
2. Surface area; it is proportional to the extracted quantity of material.
3. Diffusion resistance; it depends on the size of the particles, the porosity and the
penetrability of the extraction material for the solvent. The diffusion resistance should be
as low as possible.
4. Temperature; The higher the temperature, the better the performance of the extraction.

Extraction can be done at different pattern as follows

1. Cross flow; the extraction material is sprayed with fresh solvent at each stage.
2. Uni-flow; the extraction material is mixed with solvent and move continuously from stage
to stage in uni-flow pattern.
3. Counter flow; extraction material and solvent move continuously in a counter flow.

The counter flow method generally represents the optimum option. Compared to the uniflow
method, a considerably higher proportion of usable substance is transferred from the
extraction material into solvent. The concentration gradient as the driving force for the mass
transfer is utilized more effectively with the counter flow method. Cross flow method results in
even higher yields but requires a much more fresh solvent.

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DESCRIPTION OF THE EQUIPMENT

Figure 5.1. Solid-Liquid Extraction Unit

Solid-liquid extraction unit as shown in the diagram (1) has a spiral conveyor (2) to feed the
extraction material into revolving extractor in which the extraction process occurs. This spiral
conveyor can feed the solid up to 20 l/h with power consumption up to 4 W. Revolving
extractor is driven by a motor (4) with speed up to 9 h -1 and power consumption up to 0.9 W.
The solvent is then fed using several peristaltic pumps (5) into the revolving extractor. The
pump can feed the solvent at maximum volumetric flow rate of 25 l/h at 300 rpm. Solvent
(liquid), extract (liquid) and raffinate (solid residue) are charged into the tanks (6). The mode of
extraction can be changed by changing the selector valves (7) and the solvent can also be
heated using a heater (8) with power consumption of 330 W. All reading and controls are
placed in a cabinet (9).

EXPERIMENTAL PROCEDURE

Preparation of Extraction Material

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1. Add 10 L distilled water and 600 g potassium hydrogen carbonate and mix them until the
salt is completely dissolved.
2. Add approximately 4 kg of aluminium oxide grains in the above solution, make sure all
grains are perfectly immersed in solution and keep it in solution for 24 hours.
3. Take out the grains from the solution and dry it (if needed baking tray or oven can be used).

Experiment #1 : Extraction Performance for discontinuous process

1. Set the valve position V1 and V2 to 1 stage which means the solvent is pumped to the first
stage.
2. Weigh 70 g or aluminium oxide grains and add it to the cell extractor.
3. Make sure the cell extractor i.e. first stage is exactly positioned below the solvent feed.
4. Turn on process pump P1 and set the solvent flow rate of 15 l/h and turn on heating
element W1 and set the temperature of 30 oC.
5. Take the concentration reading at specific time interval (as can be seen in worksheet).

Experiment #2: Effect of solvent temperature on extraction performance

1. Make sure the filling hopper is filled with sufficient quantity of solid material.
2. Synchronize the speed of the solid feeder and the extractor so that a material depth
approximately 40 mm per cell is achieved.
3. Set the valve position V1 and V2 to 1 stage which means the solvent is pumped to the first
stage.
4. Turn on process pump P1 and set the solvent flow rate of 15 l/h and turn on heating
element W1 and set the temperature of 25 oC.
5. Take the concentration reading at specific time interval e.g. every 30 secs (as can be seen
in worksheet).
6. Increase the temperature to 30 oC once the extract concentration from previous
experiment does not increase anymore.
7. Take the concentration reading at specific time interval i.e. every 30 secs.
8. Increase the temperature to 40 oC once the extract concentration from previous
experiment does not increase anymore.
9. Take the concentration reading at specific time interval i.e. every 30 secs.

Experiment #3: Effect of solvent flow-rate on extraction performance

1. Make sure the filling hopper is filled with sufficient quantity of solid material.
2. Synchronize the speed of the solid feeder and the extractor so that a material depth
approximately 40 mm per cell is achieved.
3. Set the valve position V1 and V2 to 1 stage which means the solvent is pumped to the first
stage.
4. Turn on process pump P1 and set the solvent flow rate of 10 l/h and turn on heating
element W1 and set the temperature of 30 oC.
5. Take the concentration reading at specific time interval i.e. every 30 secs (as can be seen in
worksheet).

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6. Increase the flow rate to 15 l/h once the extract concentration from previous experiment
does not increase anymore.
7. Take the concentration reading at specific time interval i.e. every 30 secs.
8. Increase the flow rate to 20 l/h once the extract concentration from previous experiment
does not increase anymore.
9. Take the concentration reading at specific time interval i.e. every 30 secs.

Experiment #4: Influence of number of stages on extraction performance (optional)

1. Make sure the filling hopper is filled with sufficient quantity of solid material.
2. Synchronize the speed of the solid feeder and the extractor so that a material depth
approximately 40 mm per cell is achieved.
3. Set the valve position V1 and V2 to 1 stage which means the solvent is pumped to the first
stage.
4. Turn on process pump P1 and set the solvent flow rate of 15.5 l/h and turn on heating
element W1 and set the temperature of 30 oC.
5. Turn on process pump P2 and P3. Adjust the speed in such a way that as few air bubbles as
possible occur in the relevant intake line.
6. Take the concentration reading at specific time interval i.e. every 30 secs (as can be seen in
worksheet).
7. Set the valve position V1 and V2 to 2 stage which means the solvent is pumped to the first
and second stage.
8. Keep the setting on process pump P1 the same as step #4.
9. Turn on and adjust the speed of process pump P2 and turn on heating element W2 and set
the temperature of 30 oC.
10. Take the concentration reading at specific time interval i.e. every 30 secs (as can be seen in
worksheet).
11. Set the valve position V1 and V2 to 3 stage which means the solvent is pumped to the first,
second and third stage.
12. Keep the setting on process pump P1 the same as step #4 and that on process pump P 2 as
step #9.
13. Turn on and adjust the speed of process pump P3 and turn on heating element W3 and set
the temperature of 30 oC.
14. Take the concentration reading at specific time interval i.e. every 30 secs (as can be seen in
worksheet).

REFERENCES

Geankoplis,C.J., “Separation Processes and Unit Operations, 4th edition, Prentice-Hall Inc., New
Jersey, 2004

”CE 630 Solid Liquid Extraction”, GUNT, 2012.

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 WORK SHEETS

Experiment #1 : Extraction Performance for discontinuous process

Solvent flow rate : l/h
o
Solvent temperature : C
Time,s Conc., g/l Time,s Conc., g/l Time, s Conc., g/l Time, s Conc.,g/l
0 150 360 630
15 180 390 750
30 210 420 870
45 240 450 1000
60 270 480 1360
90 300 510 1720
120 330 570 2000

Experiment #2 : Effect of solvent temperature on extraction performance

Solvent flow rate : l/h
*indicate when you start to change the temperature.
Time,s Cond-4 Time,s Cond-4 Time, s Cond-4 Time, s Cond-4
0 1170 2340
30 1200 2370
60 1230 2400
90 1260 2430
120 1290 2460
150 1320 2490
180 1350 2520
210 1380 2550
240 1410 2580
270 1440 2610
300 1470 2640
330 1500 2670
360 1530 2700
390 1560 2730
420 1590 2760
450 1620 2790
480 1650 2820
510 1680 2850
540 1710 2880
570 1740 2910
600 1770 2940
630 1800 2970
660 1830 3000
690 1860 3030

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 720 1890 3060
750 1920 3090
780 1950 3120
810 1980 3150
840 2010 3180
870 2040 3210
900 2070 3240
930 2100 3270
960 2130
990 2160
1020 2190
1050 2220
1080 2250
1110 2280
1140 2310

Experiment #3 : Effect of solvent flow rate on extraction performance

o
Solvent Temperature : C
*indicate when you start to change the flow rate
Time,s Cond-4 Time,s Cond-4 Time, s Cond-4 Time, s Cond-4
0 1170 2340
30 1200 2370
60 1230 2400
90 1260 2430
120 1290 2460
150 1320 2490
180 1350 2520
210 1380 2550
240 1410 2580
270 1440 2610
300 1470 2640
330 1500 2670
360 1530 2700
390 1560 2730
420 1590 2760
450 1620 2790
480 1650 2820
510 1680 2850
540 1710 2880
570 1740 2910
600 1770 2940
630 1800 2970

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 660 1830 3000
690 1860 3030
720 1890 3060
750 1920 3090
780 1950 3120
810 1980 3150
840 2010 3180
870 2040 3210
900 2070 3240
930 2100 3270
960 2130
990 2160
1020 2190
1050 2220
1080 2250
1110 2280
1140 2310

Experiment #4 : Effect of number of stage on extraction performance

o
Solvent Temperature : C
*indicate when you start to change the flow rate
Time, Cond Cond Cond Time, Cond Cond Cond Time Cond Cond Cond
s -2 -3 -4 s -2 -3 -4 ,s -2 -3 -4
0 1170 2340
30 1200 2370
60 1230 2400
90 1260 2430
120 1290 2460
150 1320 2490
180 1350 2520
210 1380 2550
240 1410 2580
270 1440 2610
300 1470 2640
330 1500 2670
360 1530 2700
390 1560 2730
420 1590 2760
450 1620 2790
480 1650 2820
510 1680 2850
540 1710 2880

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 570 1740 2910
600 1770 2940
630 1800 2970
660 1830 3000
690 1860 3030
720 1890 3060
750 1920 3090
780 1950 3120
810 1980 3150
840 2010 3180
870 2040 3210
900 2070 3240
930 2100 3270
960 2130
990 2160
1020 2190
1050 2220
1080 2250
1110 2280
1140 2310

Student tasks:

1. Plot concentration (yE, g/L) against time (t, sec) for every experiment. Separate the plot if there
is change in parameter such as temperature or flow rate. Comment on the plots.
2. Do material balance for the solid-liquid leaching once the system reach steady state (experiment
#2 and #3)

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 EXPERIMENT #07 (UO-07)
PARTICLE SIZE ANALYSIS (SIEVING) and ANGLE OF REPOSE
OBJECTIVE:

1. To determine and analyze the size distribution of a fixed granular solid

2. To determine the natural angle of repose for a specific materials.

THEORITICAL BACKGROUND

Small particle is one of chemical engineering interest. An understanding of the characteristics of

masses of particulate solids is necessary in designing processes and equipment for dealing with
streams containing such solids.

One way to distinguish the particle size is by sieving. In each test sieve consists of a woven wire
screen with square apertures of known size and is used for the measurement of particle size.
The necessary vibrating motion is imparted by a mechanical shaker to ensure reproducible
results in a relatively short time.

Particle size may be specified by quoting the size of two screens, one through which the
particles have passed and the other on which they are retained. However sieving is usually used
to measure size distribution. The results of sieve test may be presented in a variety of ways
either in tabular or graphical form.

The other way to learn characteristics of solid material is by measuring the angle of repose. The
angle of repose is the steepest possible angle with the horizontal at which the material will
stand when piled. Moisture content of the material is often a controlling factor and the
percentage of fine material in the mass has a decided influence on the angle as the fine
materials carry the bulk of moisture. Similarly, the angle depends upon the type of material
including the shape and smoothness of the individual particles and their overall compactness.

DESCRIPTION OF THE EQUIPMENT

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EXPERIMENTAL PROCEDURE

A. Sieving Experiment
1. Weigh material e.g. sand that will be separated or graded using shaker and sieves. Use the
last container which is the one at the bottom of sieve series to make sure that the volume
of material does not exceed the volume of sieves.
2. Transfer the material to another container or beaker.
3. Put the sieve with the biggest screen size at the top and the smallest at the bottom (see fig
5.1)
4. Set shaker time to 20 min to make sure the material is completely graded.
5. Carefully detach each sieve and weigh the collected material from each sieve.
6. Record the mass obtained from each sieve in the work sheet.
7. Repeat the experiment twice.

B. Angle of Repose in a Hele-Shaw Cell

1. Place test material (dry or wet) in the funnel.
2. Measure the angle of repose by sliding the cell and repeat.
3. Empty the Hele-Shaw Cell by rinsing with water if required.
4. Ensure dry berfore refilling the system with another material
5. Repeat the experiment 2 times for each type of material.

REFERENCES

Instruction Manual for CEN-MKII, Armfield.

WORK SHEETS

Run #1

Screen Average Mass, g

Opening, particle
mm diameter

Total mass

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Run #2 Run #3

Screen Average Mass, g Screen Average Mass, g

Opening, particle Opening, particle
mm diameter mm diameter

Total mass Total mass

Run Material Tested and its condition Angle of Repose

1
Average

2
Average

3
Average

1
Average

2
Average

3
Average

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 EXPERIMENT #08 (UO-08)
SEDIMENTATION
OBJECTIVE:

1. To study sedimentation process and investigate the zone occurs in sedimentation tank.
2. To study the effect of flow rate of fresh water and suspension in sedimentation process.

THEORITICAL BACKGROUND

Sedimentation is a physical process of separating suspended solid in a liquid using gravity. The
suspended solids can settle down if the size is greater than 10 m. the smaller the size the
more difficult for the solids to settle down because Brownian motion and electrostatic force
balances the gravitational force. Unless coagulant is added, it is not likely to settle down very
small particle naturally.

Figure 6.1. The Four Functional Zone of Continuous Sedimentation Process

In typical sedimentation tank, there will be four functional zones. Inlet zone is the zone where
all solid particles are well mixed and flow in the same direction as the liquid. The settling occurs
in settling zone as the liquid continue flowing to outlet zone. Most of solid particles will be
settled and collected continuously in the sludge zone.

In this experiment, to determine the actual sediment content at inlet and outlet to the
sedimentation tank, samples of the mixtures are taken. This batch system will show four
different zones as can be seen in figure 6.2. In hindered settling, particles become quite close
and the liquid is flowing upward due to displacement by settling particles. This will reduce the
particle settling velocity.

Clear water
Hindered Settling
Transition zone
Compression
zone
Figure 6.2. The four zones of Batch Sedimentation

At the bottom of sedimentation column, the particles can contact each other and indeed the
particle concentration becomes very high. The settled solids are compressed by the weight of
overlying solids and water is squeezed out while the spaces between solid particles are getting
smaller. This zone is known as compression zone. Between hindered settling zone and
compression zone there will be transition zone.

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DESCRIPTION OF THE EQUIPMENT

1. Suspension flow meter 2. Fresh water flow meter 3. Switch box

4. Bypass 5. Suspension pump 6. Suspension tank
7. Fresh water/suspension 8. Outlet 9. Sedimentation tank
mixing zone 10. Baffle plate
Figure 6.3. Sedimentation Unit

EXPERIMENTAL PROCEDURE

Preparation

1. Close fresh water, suspension and by pass valves.

2. Close drain valve of suspension tank.
3. Ensure that no hose lies in the suspension tank.
4. Fill the suspension tank with 80 L of fresh water, then add 1.6 kg of precipitated calcium
carbonate.
5. Fully open bypass valve.
6. Switch on main switch and pump switch. The suspension is now mixed by the pump.

Performing the experiment

1. Drain sedimentation tank via drain valve and rinse with fresh water.

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 2. Remove or insert baffle plate (depending upon the mode of operation: undisturbed or
disturbed sedimentation. If disturbed sedimentation is chosen then insert the baffle
approximately 400 mm from inlet weir. Set a gap of 20-30 mm between bottom of baffle
plate and base of sedimentation tank).
3. Insert plug into the inlet weir.
4. Close drain valve of sedimentation tank.
5. Carefully open fresh water valve and fill the sedimentation tank with fresh water, then set
desired flow rate.
6. Move the scale on the riser for the suspension flow meter such that the zero mark is aligned
with the water level in the riser.
7. Carefully open suspension valve and set desired flow rate (the suspension mixes with the
fresh water in the inlet chamber and flows over the inlet weir into the sedimentation tank.
8. Keep checking suspension flow meter for constant flow rate, adjust suspension valve if
necessary.
9. After 10 minutes, open the valves at both sampling points at the inlet and let the
suspension flow to sedimentation cone.
10. Collect 1000 mL of the suspension from the inlet.
11. Immediately afterwards, open the valve at the sampling point at the outlet and let the
suspension flow to another sedimentation cone.
12. Collect 1000 mL of the suspension from the outlet as well.
13. After 24 hour settling duration, read the amount of sediment in the sedimentation cones
and compare (you can use flashlight to shine the sedimentation cone to enhance reading).

REFERENCES

HM 142 Gunt Experiment Manual.

NOTATION

WORK SHEETS

Time Fresh water Suspension flow Amount of Amount of Calculated amount

flow rate in rate in l/min sediment in sediment in of sediment in
l/h sedimentation sedimentation sedimentation tank
cone at inlet in cone at outlet in in ml
ml ml
100 0.5
100 1
100 2
200 2
400 2

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