4 - Unit Operations Laboratory Manual

Northern Border University
Faculty of Engineering
Chemical and Materials Engineering Department
ChE435
Unit Operations Of Chemical Engineering
Laboratory
Lecturer Eng: Abdelnasser Al-hourani
3
Table of contents
Experiment 1: Diffusion in Solution ....1

Experiment 2: Diffusion in Gases ....6
Experiment 3: Sedimentation..11
Experiment 4: Fluidized Bed Formation.....18
1- Preparing the Experiment.......22
2- Measuring Pressure Loss With Airflow.....25
3- Measuring Pressure Loss With Water flow...27
Experiment 5: Water Cooling Tower......32
Experiment 6: Reverse Osmoses ....................................................42
Experiment 7: Liquid Liquid Extraction.....57
Experiment 8: Distillation...........66
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Experiment 1: Diffusion in solution
Objective:
Direct determination of mass transfer rates in the absence of convective
effects, determination of coefficient of diffusion for liquid diffusion and
influence of absolute concentration and temperature on coefficient of
diffusion.
Apparatus:
1. The apparatus consist of:

1- Diffusion cell with capillary disc
2 - Flask
3- Agitator body
4- Magnetic agitator
5- Conductivity meter
6- Conductivity probe
2. salt
3. Distilled Water
Theory:-
Diffusion is a physical process in which a tom or molecules with in a gas, it is a form
of mass transfer.
Diffusion thus involves a flow of particles. The particles flow density
(J) Specific the number of particles that pass through a particular plane per unit of
time. It depends on the concentration gradient of the particles. This
fact in described by Fick's first law
C
J D
X
3
mol
J specific diffusion flow in
m 2 .s
m2
D Coefficient of diffusion
s
c mol
concentration gradient in direction of propagation in
x m4
The change in concentration of the diffusible particles over time is proportional to the
second derivative of the concentration in dimensions (Fick's 2nd Law) :
c C 2c

t x x
. D D
x 2
Safty Instructions:
1. Risk of electric shock :

1-1. Only technically qualified personnel may open the unit or work on the
electrical system.
1-2. Before opening the unit and working on the electrical system, completely
disconnect the unit from the mains power
1-3. Protect the electrical system against water incursion and moisture.
1-4. Electrical connections on the supply unit should only be connected when the
unit is turned off.
1-5. Never use the unit or its components for anything other than the designated
purpose.
2. Risk of injury!
2-1. Exercise caution when filling the capillary with a syringe. The sharp point of the
cannula poses a risk of serious injury.
2 2. Exercise caution when handling glass objects during experiments. Breakages
bring a risk of serious injury due to sharp glass shards.
3. Risk of damage to health!

3-1. Wipe away and dispose of any spilled or overflowed salt solution immediately.
Clean contaminated surfaces immediately.
3-2. Never use liquids or solutions other than those specified in the instructions.
3-3. Never eat or drink while performing experiments or handling the liquids or
solutions
B. Hazards to the unit and its function:
Caution 1 : Do not seal diffusion tubes or subject them to pressure . There is

a risk of bursting.
Caution 2: Do not overfill the flask and the diffusion cell. Wipe away any
spilled or overflowed salt solution immediately and clean contaminated
surfaces. There is a risk of corrosion.
3
Procedure:
1 Fill the measuring flask with 900 ml of the distilled water .

2 -Turn on the magnetic agitator with the adjusting Knob ( rest the speed to
zero )
3 Insert the conductivity probe into the measuring flask.
4 - Weigh (11.6 g) of NaCl and dissolve it completely in 200 ml distilled water
in a beaker (1 N) = 1 mol
5 Fill the diffusion cell with the experimental solution (approx... 30 ml).
(Ensure that some of the NaCl solution can remain above the capillaries).
6 Using a pipette or syringe, remove any air bubble that may remain in the
capillaries until as possible are filled with solution.
7 Turn on the a agitator at the adjusting knob and run it at between 3 and 5
revolution per sec.
8- Every 5 min take reading conductivity and record the results in the table.
Results , Calculations and Graphs:
time Conductivity Temperature

(min ) s T in c 0
k in
cm
0
5
10
15
20
25
30
35
40
45
50
60
65
70
1- Draw the relation graph between conductivity and time.

2- Calculate the difference quotient from the conductivity and experiment time
from the linear area of the measuring curve.
3 Use this data to calculate the coefficient of diffusion (D) using equation:
3
4VX k
D .
N d c2c1cs t
Where:
D: Coefficient of diffusion ( m2 / s ) .
: 3.14
V: Volume of solution with lower sink in m3, 1 litre = 1x10-3 m
X: Length of capillary in m, 5 mm = 5.0 x10-3 m
N: Number of capillaries 253
d c : Capillary diameter 1 mm = 1.0 x10-3 m
c1: Molarity of solution 1 molar
cs: Conductivity of weak solution per molarity at 20C as our measured values are
above (0.150 ms / cm .mol ) , the dilution value for 0.01 mol / dm3 has
been chosen : 111 ms/ cm. mol = 111x 105 s / cm.mol
t: time for change conductivity = final value initial value
k: Change in conductivity= final value initial value
k / t: Change in conductivity of sink over duration of experiment in s/ m.s
3
Experiment 2: Diffusion in gases
Objective:
Direct determination of mass transfer rates in the absence of convective effects,
determination of coefficient of diffusion for gas diffusion and influence of absolute
concentration and temperature on coefficient of diffusion.
Apparatus:
i. The apparatus consist of these parts:

1- Electric heater 16 - Scale adjusting ring
2- Temperature sensor PT100 17 - Lens for viewing the level
3 -Diffusion capillary tube 18 - Locking screws
4 - Float switch 19 - Heater on/off switch
5- Scale for measuring the level 20- Pump on/off switch
6- Water bath tank 21- Master switch
7- Mechanism for moving the lens
8 - Air connection for the Diffusion capillary tube
9- Control unit with air pump
10- Heater connection
11- Temperature controller
12- Float switch
13 - Temperature sensor PT 100 connection
14- Mains connection
15- Focus ring
ii. Acetone.
iii. Distilled Water.
3
Safety Instructions :
A. Risk of death or injury
1- Risk of electric shock :

1-1. Only technically qualified personnel may open the unit or work on the
electrical system.
1-2. Before opening the unit and working on the electrical system, completely
disconnect the unit from the mains power
1-3. Protect the electrical system against water incursion and moisture.
1-4. Electrical connections on the supply unit should only be connected when the
unit is turned off.
1-5. Never use the unit or its components for anything other than the designated
purpose .
2- Risk of injury!
2-1. Exercise caution when filling the capillary with a syringe. The sharp point of
the cannula poses a risk of serious injury.
2-2. Exercise caution when handling glass objects during experiments.
Breakages bring a risk of serious injury due to sharp glass shards.
3 - Risk of damage to health!

3-1. Wipe away and dispose of any spilled or overflowed salt solution immediately.
Clean contaminated surfaces immediately.
3-2. never uses liquids or solutions other than those specified in the instructions.
3-3. Never eat or drink while performing experiments or handling the liquids or
solutions
B. Hazards to the unit and its function:
Caution 1: Do not seal diffusion tubes or subject them to pressure. There is a
risk of bursting.
Caution 2: Do not overfill the flask and the diffusion cell. Wipe away any
spilled or overflowed salt solution immediately and clean
contaminated surfaces. There is a risk of corrosion.
Caution 3: Do not run the air pump when the hose is closed or
kinked. If you do, you risk damaging the pump
Procedure:
1- Connect the control unit to the heater, the Temperature sensor, float switch,
2 Fill the flask with distilled water until the float switch has definitely been
connected.
3- Fill the diffusion capillary tube with acetone until the distance from the lower edge
of the T piece to the acetone level is 40 mm (starting condition).
4 Connect the hose from the control unit to the diffusion capillary tube.
3
5 Insert the diffusion capillary tube into unit in such a way that the diffusion
capillary tube with the acetone is exposed to the temperature in the water bath.
6 Turn on the air pump using the control unit.
Results, Calculations and Graphs:

Prepare a table for recording the measured value
Time, Acetone Change in Difference Temperature

Level, Level, Quotient Water bath,
o
Sec mm L t C
L
1 Calculate the difference quotients for the change in level and the measured time.
2 Plot the change in acetone level against the difference quotient
(t / L ) in graph .
3 Use linear regression analysis to determine the gradient of the straight lines. Not
the quality of the regression analysis, the coefficient of determination R. The
maximum achievable coefficient of determination is 1.0. The values should be in
the range of 0.85 to 1.0. (The graphical representation and evaluation using
linear regression analysis of the data has been carried out using Excel).
4 Determine the K factor from the gradient.
(after draw the graphical relation between ( L ) and ( t / L ) , from graph
calculate m value: y = mx + b
m
K
2
m slope
5 Calculate the coefficient of diffusion D using the formula:
3
KRT
D
1 y0
MP ln
1 yL
kg
Mass density of acetone 789.8
m3
J
R = 8.3145 R= General gas constant
gmol .K 0
T = 313 k T = 40 + 273 = 313K
kg
M = Molar mass of acetone 0.0581
gmol
P = pressure in system= 101300 pa .
Pv = partial pressure of acetone at 40 C = 56000 pa
p
y0 v
p
y0 0.553
yL 0
3
Experiment 3: Sedimentation
Objective:
Determination of the settling speed of a particle in the suspension, settling time, and
settling performance.
Apparatus : -
1- Solid material (sand).

2- Stop Watch
3- Liquid (Water)
4- Vessels.
5- Mass balance.
Theory:
Sedimentation signifies the separation of a solid liquid suspension by means of

gravity. The action of separation utilizes the difference in density between solid
matter and liquid. The solid matter settles on the base of the sedimentation container
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with a settling speed (VA) after a settling time (t) . The magnitude of the settling speed
and the settling time is dependent on the following factors:
1 - Difference in density between the solid matter and the liquid
2 - Particle diameter of the solid matter
3 - Particle shape of the solid matter
4 - Portion by volume of the solid matter in the suspension
5 - Viscosity of the liquid
Settling Speed and Settling Time:
The sink speed can be derived approximately from the force equilibrium on the
particles of solid matter. For spherical particles this is:
4.dT . s L .g
V0
3 . L
S = Density of solid matter

L = Density of liquid
dT = Particle diameter of a spherical particle
= Drag coefficient
The determination of the drag coefficient is dependent on the Reynolds number
Turbulent Area 0.2 Re 105 0.44
Transition Area 0.2 Re 500 18.5

Re0.6
For Reynolds numbers smaller than 0.5, the equation for sink speed simplifies to
Stocks speed equation:
dT2 . S L .g
V0
18L
Where L defines the dynamic viscosity of the liquid.

The Reynolds number is defined by the following equation:-
dT .V . L
Re
L
V= Flow speed
In the industrial application of sedimentation, experience has shown Re values < 0.5.
3
To take into account the influence of the particle shape and mutual hindering by other
particles, the settling speed is determined as follows:-
VA .K .V0
= shape factor for spherical shape is 1

K = concentration coefficient
K
1 S .L
Su
s = portion by volume of the solid matter

su = Apparent viscosity of the suspension
su L 1 4.5 s for s 0.4
For the settling time (t) the following applies:
h h
t VA
VA t
h= Height of the clear column of liquid above the sediment

.
V The settling performance can be found:
. A.h
V VA . A
t
A= Area of the base of the settling container.
Notes:
Before starting the procedure it is ensured that: On the selection of the solid matter or
the liquid for the suspension, it is to ensure that:
1 - The difference in density between solid matter and liquid is sufficiently large.
2 - The solid matter has a particle size of not less than 0.5 m.
3- The liquid used does not have an effect on the properties of the material used for
the sedimentation containers or damage the material.
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4 - During this process it is to be ensured that the concentration of solid matter does
not exceed 300g/l of suspension.
5- During this process the measured mass of solid matter is placed in the measuring
beaker and the beaker filled with liquid to the 2000ml mark. The measuring beaker
is to be filled whilst being continually stirred to ensure that the solid matter is
evenly distributed in the liquid without the formation of lumps.
The experiment instructions, particularly the safety instructions, are to be read
carefully prior to set up of the unit. Prior to the start of an experiment, the participants
are to be briefed on safety aspects and the correct usage of the unit
A. Hazards for Life and Limb:
1- Danger risk of an electric shock!

1- 1. Only qualified personnel are to open the rear panel and make changes to the
electrical system
1-2. prior to opening the rear panel and working on the electrics unplug from the
mains.
1-3. Protect the electrical system from water and moisture.
B.Hazards for Unit and Function :

Attention 1:
Do not fill sedimentation containers with liquids that attack or damage plastics. The
containers will be rendered unusable by these liquids. Preferably use water.
Attention 2:
On setting up the studies apparatus, it is to be ensured that the ventilation openings on
the side of the studies apparatus remain free so that overheating in the lighting
housing is prevented.
Procedure : -
1 - Remove the sedimentation container from the container centering fitting.
2 - Fill the sedimentation container with the suspension for the experiment up to the
max. Possible mark and then close the container.
3 - Evenly shake the container for approx. 1 to 2 min. to achieve an even distribution
of the solid matter in the suspension.
4 - Quickly place the container in the container centering fitting, whilst continuing to
shake it, and fix in place (see Fig. 1). Start recording the time from the moment
that the container is positioned on the spacer block.
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5 - At regular intervals read and note the height h1 of the separation boundary
between clear liquid and cloudy suspension, and the height h2 of the particles of
solid matter settled on the base (h1 + h2 see Fig. 2).
The experiment is complete when all the solid matter has settled on the base, or it
is clear that complete sedimentation will take an inappropriately long time.
During the performance of the experiment, it is to be ensured that unintentional
knocking or vibration of the studies apparatus is avoided. Otherwise there is a
risk of incorrect measured values. On planning the experiment, it is
recommended to repeat the sedimentation experiments several times to exclude
any measuring error.
Resultes , calculations and graphs : -
Sedimentation Experiment Working : -

Solid Matter: Liquid :-
Name: - Name :-
Density: Density :-
Particle Size Range :- Dynamic viscosity :-
Particle Shape:-
t (s) h1 (m) h2 (m ) h0 - h1 VA (m /s ) V 0 (m3/ s )
1- calculate the Settling speed ( V0 ) of an unaffected spherical particle [m/s] :

-
dT2 . S L .g
V0
18L
2- Calculate the Settling speed (VA) of a particle in the suspension (affected)

[m/s]:
VA .K .V0
3
3- Calculate the Settling time [s] :
h h
t VA
VA t
4- calculate the settling performance ( m/s ) : -
. A.h
V VA . A
t
5 - Draw the graphical relationship between h (mm) and t (min).
3
Experiment 4: Fluidized Bed Formation
Objectives:
1. Observation of the fluidization process

2. Influence of the particle size on the fluidization process
3. Fluidization process in different media (air and water)
4. Fluid permeability of the solid mass and also the fluidized bed
5. Height of the fluidized bed
6. Pressure required for varying flow rates for separation of mixtures of varying
particle sizes.
Apparatus:
1. Table support with panel 16. Bypass valve for water

2. Bypass valve for air with sound absorber 17 Water supplies
3
3. Rotameter for air with needle 18, 20 Sintered plate (not visible)
4 Single tube manometers for differential air pressure 19, 21 Distribution chamber
5 Switch for diaphragm compressor 22 Air supply
6 Test vessel for air 23 Supply tank for water with drain
7 Air filter further components are behind 24 Diaphragm pump
8 Scale the cover and not visible: 25 Compressed air reservoir
9 Water overflow 26 Diaphragm compressor
10 Fixing for the upper Sintered plate
11 Test vessels for water tap and safety valve
12 Bleed / vent valve
13 Two tube manometer for water pressure
14 Switch for diaphragm pump safety valve
15 Rotameter for water with needle valve
(Theory :
In fluidized beds, granular solid matter is held in suspension by a fluid flowing

through it. As a result the solid matter takes on the character of a liquid. This relates
both to its fluid-mechanical and its thermodynamic properties.
Fluidized beds are in wide use in industry, e.g.:
Tempering baths with even temperature distribution
Powder coating
Drying plant
Furnaces
A fluidized bed is a layer of fine granular solid matter (mass) that is loosened by a
fluid flowing through it to such an 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 is set in motion and reaches a fluidized 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. Fluidized beds are widely used in process
technology.
Gaseous and sol id or liquid components of a chemical reaction are well mixed and
brought into close contact with each other. This also applies to fluidized bed furnace
applications that incinerate problem materials with low levels of pollution.
Pressure Losses in Fluidized Beds:

From the equilibrium of drag, weight and lift, the pressure loss of a fluid flowing
through the turbulent mass of particles is given by

P g 1 f h ps
p

f Density of the fluid,
p Density of the particle,
3
ps Density of the particle mass,
h Height of the mass.
Pressure Curve in the Fluidized Bed:

The equilibrium of drag, weight and lift not only applies at the base, but at any height
in the mass.
As can be seen in the previous section, the pressure loss is linearly dependent on the
height of the mass. Thus the pressure curve drops linearly to zero from the base to the
surface. With y as the immersion depth in the mass, the following applies
P
Py y
h
Loosening Speed:
This is the fluid speed at which the mass of solid matter passes the transition to a
fluidized bed.
The speed of the fluid in the space between the particles can be calculated from
Reynolds number, the diameter of the particles and the kinematic viscosity of the
fluid.
Re lo
w lo f
dp
Wlo = Speed of the fluid between the spherical particles,
Relo = Reynolds number of the fluid
dp = Diameter of the particle
f = Kinematic viscosity
As the calculation of the fluid speed applies to spherical particles, the speed for
particles of irregular shape must be corrected using a form factor
w w lo
= form factor
W = Corrected speed of the fluid
The voids fraction defines the size of the fraction of hollow space in the mass. It is
calculated from the density of the particle material and the mean density of the mass
s
1
p
= Voids fraction
The equilibrium of pressure loss and particle drag yields a relationship between the
dimensionless numbers Re and Ar
3
Re lo 42.861 1 3.11 10 4
Ar 1

1 2

3
Ar Archimedes Number
The Archimedes Number Ar is calculated from the density, particle diameter and
viscosity of the fluid
g . d p3 p f
Ar
v2 f
WARNING
Exposed electrical connections at open rear.
Risk of electric shock.
1. Disconnect from the mains supply before opening.
2. Work should only be performed by qualified electricians.
3. Protect the unit against moisture.
NOTICE (1)
Particles from the fluid bed must not enter the water tank, as the diaphragm of the
pump will be damaged if it draws in solid matter.
NOTICE (2)
Do not over exceed the measuring range of the single tube manometer, as otherwise
measuring liquid will enter the test vessel.
NOTICE (3)
Do not operate the pump or compressor against a closed valve for too long, as
otherwise the drive motor will be overloaded.
NOTICE ( 4 )
Do not fill the test vessel with materials that attack or damage plastics. The test vessel
will be rendered unusable if such materials are used.
NOTICE ( 5 )
Only operate the unit in dry rooms indoors in which there are no flammable or caustic
gasses, vapors or dusts.
Experiments
The Experiment consist of 6 parts : -
Part (1):
1. Preparing the Experiment:

1. Place the unit on a flat bench top.
2. Connect to power supply.
3. Fill the storage tank with water (approx. 4 Liter).
4. Secure all hoses at the designated points.
5. Open the bypass valves for air and water.
6. Close the needle valves on the rotameters.
3
7. Start the compressor with the relevant switch and check the function (delivery
noise).
Start the pump with the relevant switch and check the function (test vessel fills with
water
1-1. Filling the Test Vessels :-
Before experiments, the test vessels must be filled with the required mass. To practice
using the unit, we recommend initially using one of the two specimen materials
supplied. These are glass beads (ballotinis) with two different particle sizes and bulk
densities.
kg
dp = 0,180 - 0,300mm, s 1500
m3
kg
dp = 0,420 - 0,590mm, s 1500
m3
kg
The particle density for both is: = 2400...2600
m3
The air filter must be removed from the test vessel for air to fill it with the bulk
material. The water vessel must be filled in very small doses to achieve the desired
material depth. The particles sink very slowly in the water, which means that the
depth of the material can only be seen some time after filling.
1-2. Emptying the Air Test Vessel:
1. Detach all hoses on the test vessel.

2. Unscrew the knurled screws (2) at the clamp (3).
3. Remove the cylinder with the air filter and holder (1).
4. Remove the knurled screws (4) on the air filter. Caution when removing.
Maintain the seal.
5. Empty the cylinder. To loosen adherent material, tap on the cylinder while
simultaneously turning it.
6. Blow clear the pores in the sintered plate using compressed air through the
distribution chamber connection.
Adherent material can be detached from inside with a jet of compressed air.
1-3. Cleaning the Air Filter:
If the air filter is clogged up by particles carried along, it must be cleaned as follows.
1. Remove the air filter as described in part .1.2.
2. Beat the air filter on a solid surface. Material beaten out can be returned to the
solid mass.
3. Blow out the air filter from outside with a compressed air jet.
1-4. Emptying the Water Test Vessel:
The test vessel is removed in a similar way to that described in part .1.2 for the air test
vessel.
3
1. Detach all hoses on the test vessel.
2. Unscrew the two knurled screws to remove the water overflow.
3. Detach the water overflow.
4. Detach the two nuts on the retaining plate and remove the retaining plate
upwards.
5. Unscrew the two knurled screws at the clamp for holding the test vessel.
6. Empty the cylinder. To loosen adherent material, tap on the cylinder while
simultaneously turning it.
7. Blow the pores in the sintered plate clear with compressed air through the
distribution chamber connection. Adherent material can be removed from
inside with a compressed air jet.
8. Particles that are not removed from the wall by compressed air can be
removed by half filling the cylinder with water and then lightly shaking it. The
particles can be separated from the liquid with a fine filter (coffee filter).
1-5. Plotting a Calibration Curve for Recording the Pressure Losses without
filling the test vessel : -
To record the individual pressure losses for the water test vessel, a calibration curve
must be plotted for each device without filling. Make sure that no air bubbles form on
the sintered metal as they falsify the measured results.
Procedure: -
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 with
the venting and bleed valve.
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. Continuously note the flow rate and differential pressure in the table.
7. Continue the measurements up to the maximum flow.
Q L / min 0 0.2 0.3 1.9
p mmWG
m 3
W 10
s
Calculations and graphs :-

1- Draw the graphical relation between p (pressure difference through sintered
L
metal plates in mm wc) and flow rate Q in
min
The measurements with the water test vessel must be corrected with the calibration
curve you have plotted yourself. This means that the pressure
3
loss value through the sintered metal plates at the corresponding flow rate must be
subtracted from the pressure difference values from the experiments. The
measurements in this manual are corrected.
part (2):
2) Measuring the Pressure Loss with Air Flow:
2.1) Experiment Aim :-
Measuring the pressure loss with air flow with a mass with a mean particle diameter
of
dp = 0,240mm.
The mass depth is h = 50mm.
2.2 ) Performing the Experiment :-
The pressure connections are connected to the single tube manometer.

3. Turn on the compressor.
4. Increase the flow in small increments by opening the needle valve and
observe the mass.
5. Continuously note the flow rate and differential pressure.
6. As soon as the first signs of particle movements appear, the loosening speed
has been reached. Note the associated flow. Repeat the measurements until a
flow of 30 L \min is reached. Above a certain value, the flow rate can only be
increased by closing the bypass valve.
2.3) Evaluation of the Experiment:-

Put the results in the following table :-
Q L\min
1 2 3 4 5 5.5 6 10 20 30
p mmWG
rising
m 3
W 10
s
The second row specifies the speed associated with the flow. It is calculated using the
cross-section of the cylinder with Az = 15,21cm2 and the flow Q in as:
Q m
w in
6 AZ s
3
Draw the graphical relation between p (pressure loss) in mm WC and w (fluid
m 3
speed in 10 m ).
s
Part (3):
3) Measuring the Pressure Loss with Water Flow :-
3.1) Experiment Aim:

Measuring the pressure loss with water flow with a mass with a mean particle
diameter of dp = 0,505mm. The mass depth is h = 100mm.
3.2 ) Performing the Experiment : -

The pressure connections are connected to the two tube manometer. The display value
can be set to the center of the manometer with the venting and bleed valve.
observe the mass.
5. Continuously note the flow rate and differential pressure.
6. As soon as the first signs of particle movements appear, the loosening speed
has been reached. Note the associated flow
Repeat the measurements until a flow of 1.5 l/min is reached. Above a certain value,
the flow rate can only be increased by closing the bypass valve .
3.3) Evaluation of the Experiment :-
Put the results in the following table : -
Q L / 0.1
min 0.15 0.2 0.25 0.3 0.4 0.6 0.8 1.0 1.5
p
mmWG
rising
m 3
W 10
s
The second row specifies the speed associated with the flow. It is calculated using the
cross-section of the cylinder with Az = 15,21cm2 and the flow Q in L/min as:
Q m
w in
6 AZ s
3
Draw the graphical relation between p (pressure loss ) in mm WC and
m
w ( fluid speed ) in 10 3 m
s
Part (4):
4) Comparing Different Masses:
4.1) Experiment Aim:

The comparison of different masses in the air test vessel is initially carried out using a
mass with a mean particle diameter of dp = 0,240 mm.
The mass depth is h = 50mm. The experiment is then repeated with a mean particle
diameter of dp = 0,505 mm.
4.2) Performing the Experiment:

The pressure connections are connected to the single tube manometer.
3. Turn on the compressor.
observe the mass.
5. Continuously note the flow rate and differential pressure. The compressed air
flow rate is increased until the differential pressure is constant. The maximum
pressure loss is noted.
4.3) Evaluation of the Experiment : -

It can be seen that, despite different particle sizes, the maximum differential pressure
is the same for both masses. The measured maximum pressure loss for both beds is
p = 72mmWC. This measured value is now compared with the theoretical value.
According to Formula:

P g 1 f h ps
p

kg
Bulk density s 1500
m3
kg
Particle density p 2500 =
m3
kg
Fluid density f 1.25
m3
Material depth h = 0,05m
Part (5):
3
5) Determination of the Loosening speed:
5.1) Experiment Aim:-

Determination of the loosening speed from the results of the experiments in part 2 and
part 3
5.2) Performing the Experiment:

The flow speeds at which the first movement within the mass is visible in the
experiments described above (5.2 and 5.3) are noted.
5.3) Evaluation of the Experiment: -

The following values were measured:
Air: dp = 0,240mm, w = 0,0603 m / s
Water: dp = 0,505mm, w = 0,0274 m / s
The measured values are now compared with the theoretical values. First of all, the
Archimedes number is calculated using Formula (4.7),. The viscosity of the air is: -
m2
16.10 6
s
for d p 0.24 mm
Calculate A r , , Re1o , W1o ( comparison this value with the

measured value of w = 0.060 m / s .
For water, the same calculation: -

6 m2
1 . 10
s
kg
And 1000 , d p = 0.505 mm gives the following value
m3
Ar , ,Relo
Comparison with the measured value of w = 0.002739 m / s
part (6):
6 ) Relationship between Flow Rate and Depth of the Fluidized Bed : -
6.1 ) Experiment Aim : -

To determine the relationship between flow rate and the depth of the fluidized bed, a
mass with a mean particle diameter of dp = 0,505mm is used. The material depth is h
= 100mm. This experiment is only possible in the water vessel as it is only here that
the depth of the fluidized bed is clearly identifiable.
6.2) Performing the Experiment: -

The pressure connections are connected to the two tube manometer. The display value
can be set to the center of the manometer with the venting and bleed valve.
3
observe the mass.
5. Continuously note the flow rate and bed depth. Repeat the measurements until
a flow of 1,5 L\min is reached. Above a certain value, the flow rate can only
be increased by closing the bypass valve.
6.3) Evaluation of the Experiment: -

Put the results in the following table:-
Q,
L/ min 0.1 0.2 0.25 0.3 0.4 0.6 0.8 1.0 1.2 1.3 1.4 1.5
H, mm
Draw the graphical relation between h ( Bed depth in mm ) and flow rate Q in L
/ min .
3
Experiment 5: Water Cooling Tower
Objective : -
Aim of the experiments : -

The aim is to investigate and understand the influence of the
1 Volumetric air flow
2 Cooling water temperature
3 Volumetric water flow
4 Packing density
on the performance parameters of the cooling tower. For this purpose the changes of
state of the humid air are shown in an h,x graph
Apparatus : -
3
The apparatus consist of :-
1- Radial fan 16- Spray nozzle
2 - Air chamber 17- Temperature/humidity sensors
3 - Water tank with heater 18 - Temperature sensor for water
4- Drain valve for water tank 19 - Hood
5- Pump 20 -Cooling column
6- Bypass with ball valve 21- Connection for temp./humidity sensor
.
7- Water filter
8 - Drain valve for supply tank 22- Digital displays
9- Regulator valve 23- Switch for heater
10- Temperature sensor 24- Main switch
11- Flow meter 25 - Switch for fan
12- Supply tank 26 - Switch for pump
13- Drain plug 27 - Connection for pressure measurement
14- Connecting hose 28- Butterfly valve
15- Moisture eliminator
Description of the unit : -
Water circuit: -
The water to be cooled is drawn from a heated water tank by a centrifugal pump and
pumped around the circuit. The water flows regularly through a water filter, which is
installed in the direction of flow and filters particles out of the water. The water filter
is installed upstream of the flow meter, thus preventing clogging of the nozzle within
the flow meter and also the nozzle at the head of the column.
Air circuit:-
The ambient air is drawn in by a fan and fed through an air chamber into the cooling
column. Here the temperature and relative humidity of the air are measured. The
turbulence of the air inside the air chamber creates an even distribution of air over the
entire cross-section of the cooling column. The volumetric air flow can be varied
using a butterfly valve at the fan outlet.
Theory: -
Industrial cooling towers are used to remove surplus heat from water. Cooling towers
with open and closed water circuits are available. Both types function as heat
exchangers based on the counter flow principle. water is sprayed into the tower from
above and distributed as widely as possible using baffles. Ambient air is blown into
the cooling tower in the opposite direction. This causes the water to give up its latent
heat of evaporation and the air is humidified. The evaporated water must be replaced.
The cooling column is mounted on the air chamber. It is transparent, allowing the
movement of the water inside to be observed. The individual stages in the cooling
column are arranged at angles to each other, to give the maximum possible residence
time for the water. The packing density of a cooling tower is the ratio between the
total surface area of all the stages and the volume of the channel. The packing density
of the cooling column supplied with the experimental unit (type 1) is 110 m/m. The
pressure loss across the column can be measured using a pressure sensor.
3
The water to be cooled is pumped around the circuit by a centrifugal pump. The
maximum flow rate is determined by the pressure losses in the pipe system (regulator
valve, flow meter and nozzle). The flow rate can be adjusted using a ball valve on
the bypass and by a regulator valve in the main flow.
The spray nozzle is installed at the water inlet into the cooling tower. It generates a
full cone spray pattern with a square impact area. This ensures
that a fine spray of water is evenly applied to the entire cross-section of the cooling
column .
The moisture eliminator at the cooling tower air outlet consists of a kind of filter
wool, which prevents water droplets carried along with the air flow from escaping at
the top of the tower. The droplets are trapped in the fibres and fall back. This
minimizes the water loss.
The cooling load is generated by an electrical heater, which is installed in the tank.
The heater can be adjusted to 3 levels. These levels yield the following heating
capacities:
Level 1: 0.5 kW
Level 2: 1.0 kW
Level 3: 1.5 kW
The following times are required to heat the water in the tank (capacity 6 Liter ) from
20C to 40C:
Level 1: Approx. 17 minutes
The temperature is regulated using a thermostat. If the temperature exceeds 50C the
heater is turned off.
A radial fan is used to generate the air flow. It is flange mounted directly on the air
chamber. The air chamber is designed in such a way that the air passes uniformly
through the entire cross-section of the column. The volumetric air flow can be
regulated using a butterfly valve between the radial fan and the air chamber
The experimental instructions, in particular the safety instructions, are to be read
through carefully prior to operate .
Prior to operate the system, the participants in the experiment should be briefed on the
correct use of the system .
In order to ensure hazard-free operation, the following must be observed:
1) Risk of death or injury:

1-1) Danger of electric shock:
Caution when working on the electrical components of the system
There is a risk of electric shock. Disconnect the experimentation equipment from the
mains before working on it .
Have work performed only by suitably qualified personnel.
.
1-2 ) DANGER
Never operate the unit without a correctly installed earth wire ..
3
Non-compliance with this requirement means that the operator and the unit
are no longer adequately protected ..
Have the earth wire by suitably qualified person.
2) Hazards to the unit and its function:

DANGER 2-1) Never operate heater when dry.
If this is disregarded there is a risk of damage by overheating .
DANGER 2-2)
Never switch on the pump when dry. .
If this is disregarded there is a risk of damage to the pump by lack of cooling
CAUTION 2-3)
Always store the system in a dry and frost-free place .
.
CAUTION 2-4)
When cleaning, use only plastic cleaners and water ( no solvent ) .
If this is disregarded there is a risk of damage to
the plastic parts by aggressive solvents.
NOTE:
If demineralized water is used, no lime deposits Will be found during cleaning. .
CAUTION 2 -5)
The humidity sensors at the air outlet are protected by a protective tube against water
condensation on the measurement cell.
If this is disregarded the unit will display incorrect measured values.
If this happens, allow the measurement cell to dry in air.
Procedure: -
Commissioning
.
1 Fill the water tank with (6L) and the supply tank with (3L ) water .
2 Assemble the cooling column.
3 Connect the sensors: Combined temperature/humidity sensors, Temperature
sensors.
4 Connect the system to the mains electricity supply.
5 Turn on the system at the main switch and connect the unit with pc using a
ribbon cable and turn on the pc , start the software.
start Allprograms G.U .N .T WL320 The system diagram window will
appear. The start menu allows the following to be opend :-
Charts, (h,x, graph ) , system diagram ,calculation diagram , About G.U.N.T,Quit .
6 Turn on the heater and select the heating level.
level Heating time
Power(kw) min
3
1 0.5 17
2 1 8
3 1.5 6
If the temperature exceeds 50C the heater is turned off.

7- Turn on the fan; the volumetric air flow can be regulated using butterfly valve
between the radial fan and the air chamber.
8 Turn on the pump and adjust the volumetric water flow.
Assembling the cooling column

The procedure for assembling the cooling column is as follows:
Place the cooling column (2) on the air chamber (1) and secure with screws.
Place the hood (19) on the cooling column (20) and secure with screws.
Fit the connecting hose between the hood and the water supply pipe and secure it
against slipping with clamps.
Pressure loss measurement:

The pressure can be measured at three pressure tapping ports (1, 2, 3). The differential
pressure across the diaphragm at the air outlet is measured as a basis for calculating
the volumetric air flow.
PC data acquisition:
The unit is connected to the PC using a ribbon cable, which is plugged into a socket
on the left of the unit. The other end is then connected to a multi-function card
installed in a PC. When commissioning the system with PC support, it is essential to
carry out the following actions:
1. Turn on the system at the main switch.
2. Turn on the PC.
3. Start the software.
If the system is being operated without a PC, the cabling to the PC must be
disconnected, to prevent possible external signals at the sensors.
Description and operation of the WL 320 software: -

After installation, the program is called up by clicking on Start - All Programs -
G.U.N.T - WL320". The System diagram" window will appear. The Start menu
allows the following windows to be opened:
Charts
h, x graph
System diagram
Calculation diagram
About GUNT
Quit
The Language menu appears in all windows. Four languages are available.
Performing the experiment: -

The experimental system is commissioned as described in Chapter 2.6. The following
experimental settings are suggested: -
Cooling column = Type 1
3
Packing density AB = 110 m/m
Specific rain flow density R = 0.49 kg/s m2
Heating capacity =1.0 kW
To generate a heat load, all of the water in the tank should be heated to approx. 30C.
Results, Calculations and Graphs:
There are 4 types of cooling towers , will use type number 1 in the experiment .
Record the measured value in the following table:
Measuring results for cooling

column type 1
A 2
B m m3

T1 ( C0 )
1 ( % )
T2 ( C0 )
2 ( % )
T4 ( C0 )
T5 ( C0 )
P (Pa )
2 - The following values extracted using h, x graph: -

g
1- Absolute humidity ( x1 ) ,( x2 ) in ( )
kg
KJ
2- Enthalpy h1( 1 x ) , h2( 1 x ) ( )
Kg
3- Wet bulb Temperature T f 1 , T f 2 in C
4- Partial vapor pressure pD1 , pD 2 , in ( mbar )
3
m
5- Specific volume v1 , v2 in
kg
3 - The variables calculated by the pc (personal computer) are listed in below table: -
Calculated variables for cooling

column type1
kg
mL .
s
QL ( w )
Z (K )
QW (W )
a (k )
kg
m .w ( )
h
1- calculating the volumetric air flow :-
2 A22
m L P1 P2 )
.
(
A2
1 22
A
A1= a . b = (150) . (150) = 22500 mm 2 = 0.0225 m 2
D2 ( 80mm )2
A2 = 5026.5mm 2 5.0265 X 103 m 2
4 4
2- aperture ratio ( m ) : -
w1 A2
m
w2 A1
kg
3- Actual air mass flow rate ( ) : -
s
m .L . .c ( p1 p2 )
flow coefficient 0.605

exp ansion coefficient 0.98
2 A22
c
A22
1 2
A1
m3
4- Volumetric air flow ( ) :-
h
V . mL. .v f
m
5- Actual flow velocity ( ) :-
s
v.
w1
A1
6- Cooling capacity ( w ) : -
3
QL ( h2 h1 )mL.
QL QV QK
QV mL. .r .( x2 x1 )
KJ
r 2501.6
Kg.K
QK mL. c pL (T2 T1 )
KJ
C PL 1004
Kg .K
7- Calculating the heat load (w): -
QW VW. .W .C PW .(TW 1 TW 2 )
kJ
C pw 4.198
Kg.K
Kg
W 1000
m3
QW QL QV QK
mw. .c pw .(T1W T2W ) mL. .r .( x2 x1 ) mL. .C PL .(T2 T1 )
8-Calculating the wet bulub approach ( C )

a TW 2 TW 1
9- Calculating the cooling coefficient : -
Z T T
W1 W 2
(TW 1 TW 2 ) TW 1 T f 1
g L
10- Calculating the water loss ( , ) :-
s h
mw. mL. ( x2 x1 )
3
Experiment 6: Reverse osmosis
Objective :
How do you remove or reduce the molecules and ions from water using semi
permeable membrane and applied high pressure to production potable water ( RO ) .
Apparatus:
Description of device:
The complete device consists of a supply unit and a trainer. The supply unit and
trainer are connected to each other hydraulically and electrically. The installation of
the two parts of the system can be adapted to local conditions.
3
a-Process diagram
Fig (1) Process diagram
A = Membrane module , FI = Flow rate , B1 = Permeate tank

QI = Conductivity , B2 = Raw water tank , TI = Temperature
B3 = Rinse water tank , PI = Pressure , P = Pump
R = Stirring machine
3
Pump
----------------------------------------------------------------========
Tap hand operated
==============================================
Valve hand operated

==============================================
Safety valve
==============================================
Non return valve

==============================================
Pulsation damper
==============================================
Membrane
================================================
Stirrer
==================================================
Fig 2. Symbols used in the process diagram
b- Supply unit:
The supply unit contains:
3
Permeate tank B1
Raw water tank B2
Rinse water tank B3
c- Trainer:
The trainer contains all other components and control elements. It is composed:
C.1-membrane module:
The membrane module is attached to the front side of the trainer. It is a spiral wound
membrane module. It consists of the actual membrane and the pressure pipe. The
membrane is located inside the pressure pipe. The membrane separates the raw water
(salt solution) in a highly concentrated salt solution (retentate) and a low concentrated
solution (permeate).
C.2-Pump and engine:

The pump is located in the lower part of the trainer. The pump is a piston pump. It
generates the high pressure necessary for separation. An engine drives the pump.
Engine and pump are connected to each other with a V-belt. The V-belt is located
under a cover, for safety reasons.
C.3-Pulsation dumper:
The pulsation damper is located in the lower part of the trainer. It is integrated on the
pressure side of the pump. In the pulsation damper there is a membrane pre-stressed
with nitrogen.
C.4-Safety valve:
The safety valve is located in the lower part of the trainer. It is integrated on the
pressure side of the pump, behind the pulsation damper. The safety valve protects the
trainer from being destroyed by too high pressures. When the response pressure is
exceeded, the safety valve opens and liquid is released outside via the pressure relief
line.
C.5-Display and control elements:

The following electrical/electronic display and control elements are present on the
control cabinet:
1-Flow rate of the permeate FI(2) and the retentate FI(4)

Display in L/min
2-Pump P
On/off switch
3-Measuring device for conductivity

The measuring device for conductivity and temperature consists of the following
components:
Measuring transducer
Selector switch with positions for selecting the measuring point:
- QI(1) / TI(1) in the raw water
3
- QI(3) / TI(3) in the permeate
- QI(5) / TI(5) in the retentate
Connection sockets for sensors
Theory :
(RO) is a water purification technology that uses a semipermeable membrane.
This membrane technology is not properly a filtration method. In reverse osmosis,
an applied pressure is used to overcome osmotic pressure, a colligative property,
that is driven by chemical potential, a thermodynamic parameter. Reverse osmosis
can remove many types of molecules and ions from solutions, and is used in both
industrial processes and the production of potable water. The result is that
the solute is retained on the pressurized side of the membrane and the
pure solvent is allowed to pass to the other side. To be "selective", this membrane
should not allow large molecules or ions through the pores (holes), but should
allow smaller components of the solution (such as the solvent) to pass freely .
Dilute concentrated
Reverse Osmosis Osmotic pressure
Working Principle :
An applied pressure to the concentrated side the water flow transfer to the pure
side , pure solvent is allowed to pass to other side R.O can removed many types
of molecules and ions from water ( solutions) to production potable water.
How do you reduce or remove the TDS in your water?
1. Carbon Filters: (very slight reduction)

2. Reverse Osmosis (R.O.): (extremely high reduction and great tasting water)
3. Distillation : (total reduction - flat taste)

4. DI Deionization (usually a final polishing filter following a RO Reverse Osmosis
filtration system to eliminate TDS)
3
RO Removes Ionic , Nonionic , particulate , Microbiological
TYPES OF MEMBRANES:
1. Cellulose acetate
2. Polyamide hydrocarbon (PAH)
3. Sulfonated polysulfone (SPS)
Hollow fibre
Spiral bound
Tubular
RO membranes degraded by chlorine.
SPS membranes are resistant to Cl2 attack.
Chlorine-resistant membranes would eliminate the need for de-chlorination of
the RO feed and re-chlorination of permeate.
Reducing the overall cost of RO
SINGLE MODULE RO
Module : Pressure vessel containing 1 -10 RO elements
III-Experiments:
III.1-Objective of the experiment :
The following experiments investigate the influence Of:

Salt concentration in the raw water cF
Recovery Y (by varying the retentate flow rate) QR
QF = QP + QR
Flow rate of the permeate QP
Rejection R
To do this, four experiments are conducted:

Pressure in the raw water : PF= 40 bar
Retentate flow rate: Retentate flow rate:
QR= 1L/min QR= 2,5L/min
Concentration of raw 1a 1b
water: CF= 4w%
3
Concentration of raw 2a 2b
water: CF= 2,5 w%
III.2-Creating a calibration curve:
The concentrations of raw water, permeate and retentate are measured by electrical
conductivity. The conductivity is displayed on the trainer in mS/cm. To determine the
concentrations a calibration curve must be created.
To determine the calibration curve it is necessary to prepare NaCl solutions by
dilution with different concentrations. To do this, you will need a weighing scale and
several beakers (10 beakers with a volume of approximately 100 mL each and 1
beaker with a volume of approximately 1000 ml).
First of all, 2, 3, and 4g NaCl are weighed out in 3 beakers and filled with distilled
water, until the total weight of the solutions is 100g each. These are the solutions with
2, 3 and 4w% NaCl.
10g NaCl are weighed out into the largest beaker (ca. 1000mL). This is filled with
distilled water until the total weight of the solution is 1000g. This is the solution with
1w% NaCl. This solution is also used as a parent solution for diluting the other
solutions. The following three solutions are created from this solution:
0.5 w% with 50g parent solution

Distilled water is added to the stated messes of parent solution until the total weight of
each solution is 100g. Each of these solutions is diluted again by the ratio 1:10, so that
three more solutions with 0,05, 0,02 and 0.01w% are created.
safety instructions:
1) WARNING:
When the rear panel is open, electrical connections are exposed.
Risk of electrical shock.

1. Before opening the rearpanel, disconnect the plug from the power
supply.
2. All work must be performed by trained electricians only.
3. Protect the electrical installation from humidity.
2 ) WARNING:
Corrosive acids and caustic solutions
Contact with hydrochloric acid (HCl) or caustic soda (NaOH) damages the eyes and
skin. Hazardous to health if swallowed.
1. Wear protective clothing, protective gloves and protective goggles.
2. Do not swallow chemicals.
3. In case of contact with the skin, wash with plenty of water.
3
4. In case of contact with the eyes, hold eyelid open and rinse immediately with
plenty of water. Seek immediate medical attention.
5. Take note of the safety data sheet.
3 ) WARNING :
Sodium bisulphite or sodium metabisulphite
Sodium bisulphite or sodium metabisulphite can be hazardous to health. Sodium
bisulphite or sodium metabisulphite causes severe damage to
the eyes and irritates the respiratory tract. Hazardous to health if swallowed.
1. Wear protective clothing, protective gloves and protective goggles.
2. Do not swallow chemicals.
3. In case of contact with the skin, wash with plenty of water.
4. In case of contact with the eyes, hold eyelid open and rinse immediately with
plenty of water.
5. Take note of the safety data sheet.
4 ) CAUTION:
Strong noise emissions
Vibrations on the trainercan lead to strong noise emissions. Risk of hearing damage.
1. Wear ear defenders.
5 ) WARNING:
Stirring machine
The stirring machine may cause hand injuries when reaching into the raw water tank.
1. Do not reach into the raw water tank while the stirrer is rotating.
6 ) NOTICE :
Solids in the raw water will severely damage the pump and the membrane module.
1. Only use solutions for the raw water.
7 ) NOTICE:
The pump is severely damaged if operated without water.
1. Never operate the pump without water.
8 ) NOTICE:
Frost damage is possible when the device is stored.
1. Only store the system ina frost-free location.
2. If there is risk of frost or if the device will not be used for longer periods,
empty all tanks and dry them out.
9 ) NOTICE:
Screws on plastic components may not be tightened too tightly (risk of breakage).
1. Tighten the screws by hand and a maximum of one more half turn.
10) NOTICE:
Upon completion of individual experiments:
1. Clean device thoroughly.
2. Rinse equipment and hoses with fresh water or better permeate.
3. Preserve membrane in accordance with this operating manual.
3
11) NOTICE:
Do not operate pump against closed taps and valves (risk of severe damage).
1 . When operating the pump open at least one outlet tap.
Measuring procedure:
1- Remove one of the conductivity sensors QI (1), QI (3) or QI (5) from

the CE 530 trainer. To do so, the screw connection on the sensor must be
loosened and the sensor pulled out. The CE 530 trainer should be free of
pressure for this action and not filled with liquid.
2. Turn trainer on at the main switch.
3. Turn selector switch for measuring location to required position.
4. Immerse sensors one after the other into the different solutions,
beginning with the lowest concentration (i.e. with distilled water).
5. Wait a few minutes until the measured value remains stable.
6. Note down the measured value.
7. It is essential that sensors are rinsed with distilled water after each
measurement.
8. After taking all measurements, return the sensors to the bracket
on the trainer and tighten the screw connection.
9. Turn trainer off at the main switch.
Results:
Tab.1 shows sample measurement results. A chart with these measured values has
been created using a spreadsheet program (e.g. MS Excel). Spreadsheet programs
typically offer the option of adding a linear approximation function in the chart.
Please note that there is certain conductivity even at a NaCl concentration of 0%. The
reason for this is that even distilled water has a certain electrical conductivity. The
charge carriers in this case are the hydroxide and hydronium ions, which are formed
by the constant decay of water molecules. The chart with the measured values and the
approximation function are shown in Fig 3.
The linear approximation function determined in this case is:
CNaCl() = 0,0703
CNaCl : concentration w% (percent by weight)
: electrical conductivity in mS/cm
Thus the NaCl concentration can be determined a given electrical conductivity.
Table.1 Sample results for the calibration curve

CNacl (w%) Conductivity (mS/cm)
0 0,002
0,01 0,208
0,02 0,412
0,05 1,004
0,1 1,962
0,2 3,5
0,5 8,2
1 15,8
3
2 29,1
3 43,8
4 57,5
5 69,2
The linear approximation function determined in this case is:

CNaCl() = 0,0703
CNaCl: concentration w% (percent by weight)

: electrical conductivity in mS/cm
Thus the NaCl concentration can be determined a given electrical conductivity.
III.3- Conducting the experiment:

This description assumes the following initial state:
The pump is switched off.
Valve V8 is closed.
There is 24L of permeate in tank B2.
Trainer and supply unit are connected by raw water hose, retentate hose and
permeate hose
III.3.1- Experiment 1a :
1.Weigh out 1kg NaCl in a tank.
2. Turn trainer on at the main switch.
3. Turn on stirring machine R.
4. Put NaCl into tank B2 while stirring.
5. Wait until the NaCl is completely dissolved.
6. Turn stirrer off.
7. Valves and taps at the beginning:
V1 fully open V2 fully open V3 closed V4 open V5 open
V6 closed V7 closed V8 closed V9 non-return valve: nonadjustable V10
closed V11 closed V12 closed V13 closed
V14 safety valve: non-adjustable
8. Open V8.
9. Switch on the pump.
10. Put on ear defenders. Strong vibrations occur in the transition area from the
unpressurised state to the operating state,because this is out of the working range
of the pulsation damper.
11. Simultaneously turn valves V1 and V2quickly clockwise, in order to quickly
exceedthe transition area (see Fig. 5.3). Set apressure of about 40 bar.
3
12. By varying valves V1 and V2, set a flow rate of 1,0L/min in the retentate at a
constant pressure of 40bar in the raw water.
13. Wait about 5min.
14. From this point on, note down flow rates, conductivity and temperature in the raw
water, permeate and retentate every 3min.
15. The experiment ends after about 15min.
16. Do not turn pump off.
III.3.2- Experiment 1b :
17. By varying valves V1 and V2, set a flow rate of 2,5L/min in the retentate at a
constant pressure of 40bar in the raw water.
19. From this point on, note down flow rates, conductivity and temperature in the
raw water, permeate and retentate every 3min.
21.turn pump off.
III.3.3- Experiment 2a :
22. Weigh out 0,5kg NaCl in a tank.

23. Close tap V8.
24. Turn on stirrer.
25. Put (24.5L ) of permeate into tank B2.
26. Put NaCl into tank B2 while stirring.
27. Stir for ca. 1min.
28. Turn stirrer off.
29. Open tap V8.
30. Switch on the pump.
Observations:
The pressure rises immediately.
Liquid flows from the taps V4 and V5.
After strong vibrations and high noise generation in the range of 5 to 40 bar, the
vibrations drop back at 40bar.
31. By varying valves V1 and V2, set a flow rate of (1,0L/min ) in the retentate at a
pressure of (40 bar ) in the raw water.
35. Do not turn pump off.
II.3.4- Experiment 2b :
44. By varying valves V1 and V2, set a flow rate of ( 2.5 L/min )in the retentate at a
constant pressure of (40 bar ) in the raw water.
35. Turn pump off.
3
IV- analysis of the experiment:
Here, the experiments are analyzed using sample readings. The measured values are
for guidance only. The measured values vary depending on the individual reverse
osmosis modules and ambient conditions. The objective is to show:
the flow rate of the permeate ( QP ) and
the rejection R as a function of
the salt concentration in the raw water cF and
the recovery (Y )
The rejection (R ) and the recovery( Y ) must be calculated for each experiment. The
remaining valuesare given by the averages of the respective measured values.
The rejection (R ) and the recovery ( Y ) are calculated for experiment (1a ) as an
example. The others even experiments must be calculated in the same way.
The measured values of experiment (V1a ) are shown in Tab:
Permeate Retentate Raw water

Flow Cond Temp Flow Cond Temp Condt Temp
No Time rate rate
QP P TP QR R TR F TF
min L/min mS/cm C L/min mS/cm C mS/cm C
1 3
2 6
3 9
4 12
5 15
-
The averages of the measured values in the last row of Tab are used for the following
calculations.
The calculation formula for the rejection is given by:
R = Rejection in %
CP = Concentration of solute in the permeate in w%
CF = Concentration of solute in the raw water in w%
The NaCl concentrations are calculated from the average values of electrical
conductivity with Formula:
CNaCl() = 0,0703
The formula for calculating the recovery Formula is:
with QF = QP + Q R
Results in:
3
Y = Recovery in %
QP = Permeate flow rate in L/min
QF = Raw water flow rate in L/min
QR = Retentate flow rate in L/min
Rejection and recovery for the other experiments are calculated in the same way. The
following table shows a summary of the sample results.
EXPERIMENT7: Liquid- Liquid Extraction

Objective :-
The object of the experiment is to demonstrate how a mass balance performed on the
extraction column, and to measure the mass transfer coefficient and its variation with
flow rate with the aqueous phase as the continuous medium.
Apparatus: -
1. Extraction column 2. Distillation unit 3. Extract vessel

4. Feed and solvent controls
5. Control cabinet for pump operation and heater controls
6. Distillate vessel 7. Feed vessel 8. Reserve feed vessel 9. Feed pump
10. Solvent pump 11. Solvent vessel
12. Over pressure valves for pumps
13. Regulating valve for phase interface
3
14. Welded frame with castors.
Chemicals :-
1- Benzoic acid 2- petroleum Ether 3- Distilled Water .
Theory : -
Many processes in chemical engineering require the separation of one or more of the
components of a liquid mixture by treating the mixture with an immiscible solvent in
which these components are preferentially soluble. In some cases purification of a
liquid may be the function of the process, in others the extraction of a dissolved
component for subsequent processes may be the important aspect. An example of the
former is the preparation of the pure organic liquids from products of the oil industry.
Liquid-liquid extractions may also be used as energy saving processes by, for
example, eliminating distillation stages. It is possible, of course that the substance of
interest may be heat-sensitive anyway and that distillation is accordingly an
unacceptable process. When separation by distillation is ineffective or very difficult,
liquid extraction is one of the main alternatives to consider. Close-boiling mixtures or
substances that cannot withstand the temperature of the distillation, even under a
vacuum, may often be separated from impurities by extraction, which utilizes
chemical differences instead of vapor pressure differences. For example, penicillin is
recovered from fermentation broth by extraction with a solvent such as butyl acetate.
Another example for liquid extraction is recovering acetic acid from dilute aqueous
solutions; distillation would be possible in this case, but the extraction step
considerably reduces the amount of water to be distilled. When either distillation or
extraction may be used, the choice is usually distillation, in spite of the fact that
heating and cooling are needed. In extraction the solvent must be recovered for reuse
(usually by distillation), and the combined operation is more complicated and often
more expensive than ordinary distillation without extraction. However, extraction
does offer more flexibility in choice of operating conditions, since the type and the
amount of solvent can be varied as well as the operating temperature. In many
problems, the choice between the methods should be based on a comparative study of
both extraction and distillation. In liquid-liquid extraction, as in gas absorption and
distillation, two phases must be brought into contact to permit transfer of material
and then be separated. Extraction equipment may be operated batchwise or
continuous. The extract is the layer of solvent plus extracted solute and the raffinate
is the layer from which solute has been removed. The extract may be lighter or
heavier than the raffinate, and so the extract may be shown coming from top of the
equipment in some cases and from the bottom in others. The operation may of course
be repeated if more than one contact is required, but when the quantities involved are
large and several contacts are needed, continuous flow becomes economical. The
rate at which a soluble component is transferred from one solvent to another will be
dependent, among other things, on the area of the interface between the two
immiscible liquids. Therefore it is very advantageous for this interface to be formed
by droplets and films, the situation being analogous to that existing in packed
distillation columns.
Safety Instructions
The experimental instructions, in particular the safety instructions, are to be
read through carefully prior to operate the unit.
3
Prior to starting the experiments, the participants are to be briefed on the safety
aspects and the correct use of the unit.
1 ) Hazards to life and limb

1-1) Risk of electric shock:
a ) Only technically qualified personnel may open the control cabinet
or work on the electrical equipment .
b) Prior to opening the control cabinet and working on the electrical
system, unplug them from the mains .
C ) Protect the electrical equipment from water and humidity .
1-2) Danger of burns:

a ) Do not touch the hemispherical heater and glass components of the distillation
unit whilst distillation is in progress.
b) When emptying the distillation receiver: be sure to pour hot bottom product into
suitable containers. Wear protective gloves at all times.
.
1-3) Danger, health risk:
When handling the chemicals that are used, work strictly to the hazard instructions
and safety instructions described in the safety data sheets.
This applies particularly when filling and emptying the unit..
2 ) Dangers to the unit and its functionality

2-1) ATTENTION :
The unit is designed exclusively for use with the material combination petroleum
ether, benzoic acid and distilled water. If used with other material combinations, make
sure it is resistant. Only use chemicals that do not cause damage to VITON,PVDF
,PTFE and1.4035
2-2 ) ATTENTION:
Never heat the distillation round-bottomed flask , when it is empty there is risk of
overheating which can lead to embrittlement and consequent failure of the heater ..
2-3) ATTENTIONS:
The hemispherical heater is not protected against humidity. Take care therefore not to
expose it to humidity or wetting, nor to aggressive media. If the heater does become
wet, it must be fully dried out (preferably in a drying cupboard) before being used
again.
.
Procedure : -
1- prepare the feed mixture , weigh 60 gr of benzoic acid in powder form is dissolved
in ( 25 L) petroleum ether and fill the feed tank .
2 Fill the solvent tank with distilled water .
3- close the regulating valve for the phase interface and switch feed pump to pumping
the feed mixture into the bottom of the extraction tower .Allow the feed mixture to
flow continuously in a circuit .
3
4- - Switch on the solvent pump and feed solvent into the extraction column .
5- Open the regulating valve when a clear phase interface can be seen in the free
spaces of the extraction column. By regulating the feed flow and solvent flow,
using the volumetric quantity meters and the regulating valve, maintain the phase
interface at a constant height.
6 - In batch operation, allow the feed and solvent to flow in a circuit and at regular
intervals take samples from the solvent and feed vessels, for analysis of the
composition. When the desired separation has been achieved, divert the feed flow
into the reserve feed vessel and the solvent flow into the extract vessel.
7 - In continuous operation the feed and solvent are fed directly from the storage
tanks, through the extraction column, then into the receiver vessels.
8 - Where the feed mixture has a density significantly less than that of the solvent, the
height of the liquid column of feed mixture in the extraction column may be
insufficient to convey the solvent into the extraction vessel. In this case the flow
resistance at the head of the extraction column must be increased, by using the
manipulation valve (21).
9 - For emptying the unit it is necessary to pump the feed from the feed vessel into the
reserve feed vessel. The liquid can be drained from the reserve feed vessel, using the
drain valve. For the solvent, which as a rule must be reprocessed, the liquid can be
drained either from the extract vessel or the distillate vessel.
10 - To drain the extraction column open the drain valves (1) & (2) and let the liquid run
off into a suitable container. Run solvent- and feed pump as long as air is running
through the flow-meters obviously.
11 - After emptying, the unit should be washed through several times with distilled water (
run the water into suitable containers and arrange for it to be correctly disposed of ).
12 - For distillation it is necessary that the boiling temperature of the component to be

distilled is known and is entered into the PID controller using the arrow keys. Then
the rotary switch is used to set the distillation heater.
13 - For vacuum distillation the water jet pump supplied should be connected to a suitable
water supply and using the hose provided a vacuum connection made between the
distillation tube and the water jet pump.
After an extraction time of approx. 1 hour the solvent flow is switched to the extract
vessel. A measurement of the conductivity will show an increase in the electrical
conductivity of the water.
The solvent is fed from the extract vessel to the distillation unit, to distil part of the
water from the mixture. After a distillation time of 1 hour , the conductivity of the
water is measured again.
NOTES : -
3
1) The conductivity will change as follows: - .
Solvent before extraction: 0s
Solvent after extraction: 170s
Bottom product after distillation: 850s
2) In order to measure the concentration of benzoic acid in the water, the electrical
conductivity can be measured directly, to indicate the concentration.
3) The concentration of benzoic acid in the petroleum ether cannot be measured
directly. For this, a defined quantity of petroleum ether must be mixed with a
defined quantity of dist. water. After being thoroughly mixed, the electrical
conductivity of the water indirectly indicates the concentration of petroleum ether.
4) The electrical conductivity of the water increases with the concentration of benzoic
acid in the water.
calibration curve water - benzouic acid
300
250
conductivity
200
150 Series1
100
50
0
0 0.2 0.4 0.6 0.8 1 1.2
concentration
The measurements should be performed using the conductivity meter supplied. The
conductivity meter is not to learned for measuring absolute values. It is sufficiently
precise for making relative measurements indicating qualitative changes.
Results ,Calculations and Graphs :-
Feed(petroleum ether + Benzoic acid ) Solvent (distilled water )

Time Conductivity Concentration Place Time Conductivity Concentration Place
s of min s of
Min cm sampling cm sampling
0 Feed 0 Solvent
tank tank
10 Bottom 10 Top of
of Tower
3
Tower
20 20
30 30
40 40
50 50
60 60
Calculations : -
The theory for the system petroleum ether -benzoic acid-Water is as follows:
Let
Vw : Water flow rate, L/s
Vo : petroleum ether flow rate, L/s
X: benzoic acid concentration in the organic phase, kg/L
Y: benzoic acid concentration in the aqueous phase, kg/L
Subscripts: -
1 : Top of column
2 : Bottom of column
Mass Balance :
benzoic acid extracted from the organic phase (rafinate).
= v0 ( x1 x2 ) ------------------ ( 1 )
benzoic acid extracted by the aqueous phase (extract)
= vw ( Y1 0 ) ------------------- (2 )
Therefore theoretically,
v0 ( x1 x2 )= vw ( Y1 0 ) ----------------(3)
Mass transfer coefficient:
Rate of acid transfer
MTC ------ (4 )
( volume of packing ) ( Mean driving force )
Where : -
Log mean driving force :- (X1-X2) / ln (X1/X2)
X1 : Driving force at the top of the column = (X1-X1* )
X2 : Driving force at the bottom of the column = (X2-X2 *)
where X1 and X2 are the concentrations in the organic phase which would be in
equilibrium with concentrations Y1 and Y2 ( = 0.0) in the aqueous phase,
respectively. The equilibrium values can be found using the distribution coefficient
for the chemicals used (Assumed that Y = K X relation holds at equilibrium for a
constant K). Rate of acid transfer may be calculated using Eqs.( 1) or (2) based on
raffinate or extract phases, respectively.
3
1. Find benzoic acid concentrations in each stream. Calculate the average value for
each data point. Check the variances and eliminate the outliers if there are any.
Carry out the following calculations using the refined data set.
2. Calculate the mass transfer coefficients based on both phases.
3. What is the maximum possible acid transfer rate? Calculate the column efficiency
using experimental and maximum acid transfer rate. What should be done to
achieve the maximum acid transfer rate?
4. Repeat the calculations for all flow rates.
5. Try to answer the following questions in your discussion and conclusion:-
a) Why does the mass transfer coefficient depend on the phase selected as the
base?
b) How does the flow rate affect MTC? Why?
c) How can the efficiency of the column be increased?
d) Were there any source of error in the experiment? How can this experiment be
improved?
EXPERIMENT 8: Distillation
Objective :-
The range of experiments covers the following variants:

batch and continuous Distillation.
Sieve plate column and packed column.
Sieve plate column, 3 different infeed heads selectable.
Reduction in the number of plates in the sieve plate column.
Operation at atmospheric pressure or under vacuum.
Operation with or without feed preheating.
Apparatus : -
3
The Distillation unit consist of : -
1- Feed pump , 2- Feed tank, 3- Control cabinet, 4- Top product tank
5 -Glass filter pump, 6- Pressure gauge , 7- Switching valve,
8 - Phase separation tank 9 -Product condenser , 10- Switching valve
11- Differential pressure sensor, 12- Solvent tank
13- Column, 14- Flowmeter for cooling water, 15 -Evaporator
16- Bottom heat exchanger 17- Bottom product tank
Batch Distillation ( under atmospheric pressure )

Experiment aims are:
1. To concentrate the ethanol
2. To record the measured value using the data acquisition program (temperature and
pressure profiles)
3. To determine the ethanol concentration in the initial mixture, top product and
bottom product
4. To depict the change over time of the ethanol concentration in the top product
5. To check the concentrations by means of mass
The experiment instructions, in particular the safety instructions, must be read
thoroughly prior to starting up the unit. Before commencing an experiment, all
3
participants must have been instructed in the safety aspects and proper handling of the
unit.
1) Health hazards:
1-1) WARNING
Risk of electric shock when working on the control cabinet
Have work on the control cabinet carried out only by a qualified electrician. Prior to
opening the control cabinet, unplug the mains power plug.
1-2) WARNING
Risk of electric shock due to wetness and moisture on the control cabinet.
Do not allow the control cabinet to get wet.
1-3) WARNING
There is a risk of explosion if the wrong chemicals are selected. .
Select chemicals such that ignition temperatures cannot be reached during operations.
This applies to the single input materials and to mixtures of them.
1-4) WARNING
Potential health hazard when handling chemicals .
Follow the relevant health and safety instructions particularly with regard to charging
and draining the unit.
1-5) WARNING
Risk of burns by touching the apparatus, in particular the evaporator, the
column and the pipes.
Do not touch hot surfaces
1- 6) WARNING:
Risk of scalding when removing the heated bottom product.
Drain the heated bottom product only into a heatproof container, and wear heat-
resistant gloves while doing so .
2) Hazards to the unit and its function

NOTICE
The choice of chemicals for rectification is limited by the resistance of the materials
used in the construction of the equipment. Use only chemicals which do not attack
VITON, PVDF PTFE and stainless steel.
Procedure : -
Commissioning
Ensure that all hose connections are secure and free from leaks
Connect the cooling water supply and reflux lines, reflux unpressurized
Connect the unit to the mains electricity supply
Install the data acquisition and control program on the PC
Plug the unit into the PC For more information and detailed instructions.
1- NOTES before operating the unit :-

* For operation at ambient pressure it is important to open the manual stop valve (1)
underneath the pressure gauge. This equalizes the pressure relative to the atmosphere .
3
** The stop valve (3) at the feed connection of the column should be closed so as to
avoid unnecessary thermal loading on the hose.
Conditions for this experiment are:

Initial mixture 10L, ethanol fraction 25%m
packed column
Operation at atmospheric pressure
Cooling water flow 150L/h
Operation at heating power 30%, Reflux ratio 50%
Rectification aborted (heater off) on reaching evaporator temperature
T3 = 92C
Performing the experiment : -

1-.Open the manual stop valve underneath the pressure gauge.
2- The requirement is a canister containing more than 10L of initial mixture, ethanol:
25%m, water: 75%m (new addition, e.g. for 12L, with 2885g ethanol and 8655g
water).
3- Mix the initial mixture in the canister.
4 - Identify the density and temperature of the initial mixture. Check the
concentration.
5 - Transfer the initial mixture from the canister into the two feed tanks (VI). Use
measuring cups for this, and weigh the content of each cup (net weight of each).
Fill the feed tanks up to their 5litre marks. Also weigh the residue in the
measuring cup.
6 - Transfer the initial mixture from the feed tanks through the column into the
evaporator. To do so, open the stop valve on the column during pumping.
7 - Press Reset on the differential pressure display
8 - Unit operation by PC. Make the settings for data acquisition, open the measured
value file
9 - Set the reflux ratio to 100% initially
10 - Open the condenser water supply and adjust it to about 150L/h
11 - Switch on the heater. Initial fixed value 100% When evaporator temperature T3
= 70C is reached, reduce the heater to the fixed value 20%
12 - Wait for distillate to appear at the phase separation tank (IV), reflux begins and
the system reaches a state of equilibrium (temperatures constant about 20minutes
after first appearance of distillate). Then changes to operating conditions:
- Heater from 20 to 30%
- Reflux ratio from 100 to 50%
13 - When the minimum sample volume is reached, withdraw the top product from
the top product tank (V). Determine the mass, density and temperature. Keep the
sample (for a later mixed sample). Perform a new measurement as soon as the
minimum sample volume has been reached again.
14 - Abort on reaching T3 = 92C
15 - 5 minutes after aborting, change reflux ratio to 100%. Shut off the water supply.
16 - Measure the remaining top product (residue from top product tank together with
residue from phase separation tank); determine the mass, density and
temperature.
18 - Pour together and intermingle the previous top product samples and measure the
total mass, density and temperature.
3
19 - Cool the bottom product from the evaporator . Drain off the cooled bottom
product, weigh it and mix it in the second canister. Take a sample of the bottom
product mixture, determine density and temperature.
20 - Fill canister with unused initial mixture and with top and bottom product. Mix
well. This provides a new initial mixture for the next experiment.
Shutdown :-
Shut down the PC

Switch off the unit at the master switch
Shut off the water supply and isolate the unit from the water main
Leave unit to cool
Check the positions of the hand valves, prevent unintentional leakage of liquids
If the unit is being shut down for a lengthy period of time, drain all tanks completely
Results ,Calculation : -
The self-recorded measured values are primarily the masses, densities and
temperatures of the various mixtures/products. In the course of the experiment they
were entered by hand on the Batch worksheet
Measurement Evaluation
Mass
Clock Product/ Mass Temp., Density, Level, Mass fraction
measurement Net, C Net, Ethanol, ,
no. g g\ cm3 L g wE
Measurement
Start, Fill feed tank,

Individual masses in
g
End, B.pr., from
Evap,
g
3
Key: T.pr.: Top product; B.pr.: Bottom product; Evap: Evaporator
Tab. 7.1 Batch worksheet for self-recorded measurements in the Batch
experiment series To determine the ethanol concentrations:
For all the samples, the ethanol mass fraction E wE was determined from the density
and temperature by means of linear interpolation.
After getting the results in the table knowledge of the temperature and density can be
extracted mass fraction of ethanol from the attached table but if the temperature and
density is not found in the attached table can hold linear interpolation
To check the concentrations by means of mass balances
It is useful to check the measured values with the aid of mass balances. Any conflicts
arising from the mass balances indicate errors in evaluation or
inaccurate measurement data. At this point the mixture and ethanol masses at the start
and end of the experiment are compared: The following examples illustrate the
graphical symbols used below:
where : -
m: Mixture mass, general
mE: Ethanol mass, general
wE: Ethanol mass fraction, general
m(Start): Mixture mass, at start of experiment
mE(End): Ethanol mass, at end of experiment
wE(T.pr.): Ethanol mass fraction in top product
m(T.pr.): Mixture mass, top product
Mixtures mass balance:

To be checked
m(Start) = m(End) . ( 1 )
m(End) = m(T .pr.)+ m(B.pr.,Evap ) ( 2 )
Ethanol mass balance:

In line with the mass balances for the mixtures, (.1) and(.2), the resultant ethanol mass
balances are:
mE (Start ) = mE(End) ..(3 )
where : -
mE((End) = mE((T.pr). + mE(B.pr.,Evap)
The ethanol mass fraction wE is defined as the ratio of the ethanol mass mE to the
mixture mass m. This enables the individual ethanol masses to be expressed as the
product of the mixture mass and the mass fraction, e.g. for
mE (T .pr) . = m(T.pr). + wE (T.pr.) ..( 4 )
Continuous Distillation: (Atmospheric pressure)
Experiment aims:
1. To concentrate the ethanol
2. To record the measured value using the data acquisition program (temperature and
3
pressure profiles)
3. To determine the ethanol concentration in the initial mixture, top product and
bottom product
4. To present the change over time in the ethanol concentration in the top and bottom
products
5. To check the concentrations by means of mass balance
Performing the experiment :-

1 - Prepare the unit . Open the manual stop valve underneath the pressure gauge.
2 - The requirement is a canister containing more than 19L of initial mixture, ethanol:
25%m, water: 75%m (new addition, e.g. for 20L, with 4808g ethanol and 14425g
water).
3 - Mix the initial mixture in the canister
4 - Identify the density and temperature of the initial mixture. Check the
concentration.
5 - Transfer the initial mixture from the canister into the two feed tanks (VI). Use
Fill the feed tanks up to their 5litre marks. Also weigh the residue in the
measuring cup (after pumping out, pour into feed tank).
6 - Transfer 9 of the 10L of initial mixture from the feed tanks through the column
into the evaporator . While transferring, open the stop valve on the column.
Switch the pump off when the 9L level is reached according to the markings on
the feed tanks.
7 - Transfer additional initial mixture from the canister into the two feed tanks. Use
Fill the feed tanks up to their 5L marks. Also weigh the residue in the measuring
cup.
8 - Check whether the heat exchanger (VII) is switched for feed heating.
9 - Press Reset on the differential pressure display.
10 - Unit operation by PC. Make the settings for data acquisition, open the measured
value file .
11 - Set the reflux ratio to 100% initially
12 - Open the condenser water supply and adjust it to about 300L/h.
13 - Switch on the heater. Initial fixed value 100%.
14 - When evaporator temperature T3 = 80C is reached, reduce the heater to the
fixed value 25%.
15 - Wait until distillate appears at the top tube of the phase separation tank (IV) and
reflux begins. After waiting 5minutes, change operating conditions:
Start feed in column, pump (X) on at 20%
Reflux ratio from 100 to 25%
Open valve slightly from evaporator to front bottom product tank
Note down the volume in the evaporator
Keep the level in the evaporator as constant as possible, adjusting the valve
setting as necessary .
16 - When the minimum sample volume is reached, withdraw the top product from
the top product tank (V). Determine the mass, density and temperature. Keep the
sample (for a later mixed sample). Note down the volume in the evaporator.
Perform a new measurement as soon as the minimum sample volume has been
reached again.
3
17 - When the minimum sample volume is reached, withdraw the bottom product
from the bottom product tank (VIII). Determine the mass, density and
temperature. Keep the sample (for a later mixed sample). Note down the volume
in the evaporator. Perform a new measurement as soon as the minimum sample
volume has been reached again.
18 - Abort e.g. after adding 5L feed:

Pump off
Heater off
Close valve from evaporator to bottom product tank
19 - 5minutes after aborting, change reflux ratio to 100%. Shut off the water supply.
20 - Measure the remaining bottom product (totally drain bottom product tank);
determine mass, density and temperature.
21 - Pour together and intermingle the previous bottom product samples and measure
the total mass, density and temperature.
22 - Measure the remaining top product (residue from top product tank together with
residue from phase separation tank); determine the mass, density and
temperature.
23 - Pout together and intermingle the previous top product samples and measure the
total mass, density and temperature.
24 - Cool the bottom product from the evaporator . Drain off the cooled bottom
product, weigh it and mix it in the second canister. Take a sample of the bottom
product mixture, determine density and temperature.
25 - Fill canister with unused initial mixture and with top product and the two bottom
products. Mix well. This provides a new initial mixture for the next experiment.
Shutdown :-
Shut down the PC

Switch off the unit at the master switch
Shut off the water supply and isolate the unit from the water main
Leave unit to cool
Check the positions of the hand valves, prevent unintentional leakage of liquids
If the unit is being shut down for a lengthy period of time, drain all tanks completely
Results and Calculations : -
Measurement Evaluation
Mass
Clock Product/ Mass Temp Density Level Mass fraction
measurement Net C Net Ethanol ,
no. g g\ cm3 L g wE
Start,mixture,Evap
3
End,T.pr,mixture
End,B.pr,mixture
End,B.pr,Evap
Measurment
Start, Fill feed tank,
g
End, B.pr., from
Evap,
g
Key: T.pr.: Top product; B.pr.: Bottom product; Evap: Evaporator

Tab.2 Continuous worksheet for self-recorded measurements in the Continuous
experiment series
To check the concentrations by means of mass balances : -

It is useful to check the measured values with the aid of mass balances. Any conflicts
arising from the mass balances indicate errors in evaluation or inaccurate
measurement data. At this point the mixture and ethanol masses at the start and end of
the experiment are compared:
m: Mixture mass, general

mE: Ethanol mass, general
wE: Ethanol mass fraction, general
m(Start): Mixture mass, at start of experiment
mE(End) : Ethanol mass, at end of experiment
m(Evap): Mixture mass in evaporator
mE(Feed): Ethanol mass in feed tanks
wE(T.pr.): Ethanol mass fraction in top product
m(B.pr.): Mixture mass, bottom product
Mixtures mass balance:
To be checked:
m (Start) = m (End) .( 6 )
3
where: -
m ( Start) = m ( Start, Evap) + m ( Start, Feed) .( 7 )
and : -
m(End) = m ( T .pr) . + m (B .pr) + m (B .pr.,Evap) +
m(End,Feed) .(8)
Ethanol mass balance:

In line with the mass balances for the mixtures,(6) to(.8), the resultant ethanol mass
balances are:
To be checked:-
mE ( Start) = mE ( End) ... (9)
where : -
mE (Start) = mE( Start, Evap ) + mE(Start, Feed) .(10)
and
mE( End) = mE( T .pr). + mE (B.pr). + mE (B.pr.,Evap) +
mE (End , Feed) (11)
The ethanol mass fraction wE is defined as the ratio of the ethanol mass mE to the
mixture mass m. This enables the individual ethanol masses to be expressed as the
product of the mixture mass and the mass fraction, e.g. for
mE (T.pr). = m (T.pr.) x wE (T.pr.).( 12 )

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Northern Border University

Lecturer Eng: Abdelnasser Al-hourani

Experiment 1: Diffusion in Solution ....1

1. The apparatus consist of:

1. Risk of electric shock :

3. Risk of damage to health!

Caution 1 : Do not seal diffusion tubes or subject them to pressure . There is

1 Fill the measuring flask with 900 ml of the distilled water .

Results , Calculations and Graphs:

time Conductivity Temperature

1- Draw the relation graph between conductivity and time.

i. The apparatus consist of these parts:

A. Risk of death or injury

1- Risk of electric shock :

3 - Risk of damage to health!

Results, Calculations and Graphs:

Time, Acetone Change in Difference Temperature

1- Solid material (sand).

Sedimentation signifies the separation of a solid liquid suspension by means of

Settling Speed and Settling Time:

S = Density of solid matter

Turbulent Area 0.2 Re 105 0.44

Transition Area 0.2 Re 500 18.5

Where L defines the dynamic viscosity of the liquid.

= shape factor for spherical shape is 1

s = portion by volume of the solid matter

su L 1 4.5 s for s 0.4

For the settling time (t) the following applies:

h= Height of the clear column of liquid above the sediment

A= Area of the base of the settling container.

A. Hazards for Life and Limb:

1- Danger risk of an electric shock!

B.Hazards for Unit and Function :

1 - Remove the sedimentation container from the container centering fitting.

Resultes , calculations and graphs : -

Sedimentation Experiment Working : -

1- calculate the Settling speed ( V0 ) of an unaffected spherical particle [m/s] :

2- Calculate the Settling speed (VA) of a particle in the suspension (affected)

1. Observation of the fluidization process

1. Table support with panel 16. Bypass valve for water

In fluidized beds, granular solid matter is held in suspension by a fluid flowing

Pressure Losses in Fluidized Beds:

Pressure Curve in the Fluidized Bed:

1. Preparing the Experiment:

1-1. Filling the Test Vessels :-

1-2. Emptying the Air Test Vessel:

1. Detach all hoses on the test vessel.

1-3. Cleaning the Air Filter:

1-4. Emptying the Water Test Vessel:

1. Connect the pressure measuring connections to the manometer. On a two tube

Q L / min 0 0.2 0.3 1.9

Calculations and graphs :-

2) Measuring the Pressure Loss with Air Flow:

2.1) Experiment Aim :-

2.2 ) Performing the Experiment :-

The pressure connections are connected to the single tube manometer.

2.3) Evaluation of the Experiment:-

3) Measuring the Pressure Loss with Water Flow :-

3.1) Experiment Aim:

3.2 ) Performing the Experiment : -

3.3) Evaluation of the Experiment :-

Put the results in the following table : -

4) Comparing Different Masses: