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Faculty of Engineering
Chemical and Materials Engineering Department
ChE435
Unit Operations Of Chemical Engineering
Laboratory
3
Table of contents
3
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:
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:
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.
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:
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:
ii. Acetone.
iii. Distilled Water.
3
Safety Instructions :
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.
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.
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 : -
Theory:
3
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
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
For Reynolds numbers smaller than 0.5, the equation for sink speed simplifies to
Stocks speed equation:
dT2 . S L .g
V0
18L
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
K
1 S .L
Su
h h
t VA
VA t
. A.h
V VA . A
t
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.
3
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.
Safety Instructions :
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
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 : -
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.
3
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.
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:
Apparatus:
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 :
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.
3
ps Density of the particle mass,
h Height of the mass.
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
Safety Instructions :
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):
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
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.
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.
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: -
p mmWG
m 3
W 10
s
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):
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.
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):
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 .
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):
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:
part (6):
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 : -
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
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
Level 2: Approx. 8 minutes
Level 3: Approx. 6 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
Safety Instructions :
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:
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.
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
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.
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.
There are 4 types of cooling towers , will use type number 1 in the experiment .
Record the measured value in the following table:
T1 ( C0 )
1 ( % )
T2 ( C0 )
2 ( % )
T4 ( C0 )
T5 ( C0 )
P (Pa )
kg
m .w ( )
h
2 A22
m L P1 P2 )
.
(
A2
1 22
A
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 )
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
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 )
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
3
Pump
----------------------------------------------------------------========
==============================================
Safety valve
==============================================
Pulsation damper
==============================================
Membrane
================================================
Stirrer
==================================================
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.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.
2-Pump P
On/off switch
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
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.
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
III-Experiments:
QF = QP + QR
Flow rate of the permeate QP
Rejection R
3
Concentration of raw 2a 2b
water: CF= 2,5 w%
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:
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.
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:
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.
3
2 29,1
3 43,8
4 57,5
5 69,2
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.
18. Wait about 5min.
19. From this point on, note down flow rates, conductivity and temperature in the
raw water, permeate and retentate every 3min.
20. The experiment ends after about 15min.
21.turn pump off.
III.3.3- Experiment 2a :
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.
32. Wait about 5min.
33. From this point on, note down flow rates, conductivity and temperature in the raw
water, permeate and retentate every 3min.
34. The experiment ends after about 15min.
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.
45. Wait about 5min.
46. From this point on, note down flow rates, conductivity and temperature in the raw
water, permeate and retentate every 3min.
47. The experiment ends after about 15min.
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:
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.
Apparatus: -
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.
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 .
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 ).
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: - .
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.
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.
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 :-
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
Safety Instructions :
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 .
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.
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.
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 :-
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
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
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 )
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
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.
Shutdown :-
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,
Individual masses in
g
End, B.pr., from
Evap,
Individual masses in
g
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)
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