Você está na página 1de 59

# EXPERIMENT 1: PACKED BED DISTILLATION COLUMN

1.

Objective:
To operate the column under total reflux condition and calculate the minimum number of
theoretical stages using fenskes equation. To operate the column under any desired
reflux condition and calculate theoretical number of stages using Mc-Cabe Thieles
method

1
2.

Description:
The set-up consists of packed column, which is packed with glass rasching rings. An
electrically heated reboiler is installed at the bottom of the column. A tank is provided to
collect the bottom product. Shell and tube type condenser is provided to condensate the
vapour. A tank with pump and rotameter is provided for circulation of cooling water.
Reflux drum is provided to collect the condensate. Receiving tank is for collecting the
distillate. Drain valves are provided for drainage purpose.

3.

Theory
4.1

Part 1

Packed column are often used for distillation when the separation is relatively easy and
the required column diameter is not very large. The column height is generally based on
the number of theoretical plates and the height equivalent to theoretical plate (HETP).
For the calculation of height equivalent to theoretical plate (HETP):

Where Z and Nt are packed height and number of theoretical plates respectively. For
simple batch distillation process, initially the still is filled with F moles of feed with xF
as the mole fraction of the more volatile component. Let at any moment the number of
moles of liquid in the still be B having a mole fraction x of the more volatile component
(i.e A) and let the moles of accumulated condensate be D. Concentration of the
equilibrium vapour is y*. Over a small time, the change in the amount of liquid in the
still is dB and the amount of vapour withdrawn is dD. The following differential mass
balance equations may be written:

The above equation is more convenient form of rayleigh equation. Batch distillation with
only a single still does not give a good separation unless the relative volatility is very
high. To obtain product with a narrow composition range, a rectifying batch still is used
that consist of a reboiler, a rectifying column, a condenser, some means of splitting of a
portion of condensed vapor or distillate as reflux and the receiver. The operation of a
batch still and column can be analyzed using the same operating line equation as for the
rectifying section of the continuous distillation:

Since the slope of the operating line is R / (R+1), the slope increases as the reflux
increases, until when reflux is infinite. Under total reflux slope is 1. The operating line
then coincides with the diagonal. The number of plate is minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of
xB and xD based on the relative volatility of the components , which is defined in terms
of equilibrium concentrations:
Minimum number of theoretical plates required:

The above equation is known as fenskes eqn. The final ratio does not change much over
the range of temperature encountered in a typical column, so the relative volatility is
taken as constant.
4.2

Part 2

## Method to calculate number of theoretical plates (mc-cabe thieles method):

For the determination of number of theoretical plates at desired reflux ratio. We are using
graphical method which is called Mc-Cabe Thieles method. In this method draw the
equilibrium data on x-y plane. Locate the point xD, xB, and xF on diagonal. For the
given reflux ratio R calculate the intercept on the rectifying section operating line on the
y-axis. Now calculate the slope of the feed line:

## Follow the following procedure to calculate theoretical number of plates (Nt):

a) Plot the equilibrium data on x-y plane.
b) Locate the point xD, xB, and xF on diagonal.
c) Draw the rectifying line from point xD with intercept I on the y axis.
d) Also draw the feed line from the point xF with slope S and intersect the rectifying line,
that intersection point is M.
e) Now draw the stripping line from point xB to the intersection point M.
f) Draw horizontal line from the point xD to equilibrium curve.

g) Draw vertical line from the point at equilibrium curve (where horizontal line is end) to
the operating line.
h) The above step made triangular construction.
i) Again draw horizontal line from the point at operating line (where vertical line is end)
to the equilibrium curve.
j) Repeat the above three steps between equilibrium curve and operating line, till cover
the point xB on diagonal.
k) Count the number of triangles made.
l) Number of triangles is equal to number of theoretical stages including reboiler.
m) Subtract one from the number of triangle, and then it is theoretical number of stages
required at desired reflux conditions.
For the overall efficiency of the column can be use following formulae:

4.

Procedure:
4.1 Starting Procedure:
4.1.4

4.1.5

4.1.6

4.1.7

## Fill water in the cold water tank

4.1.8

Fill the reboiler with methanol-water solution by open the valve V1 and
air vent valve V2

4.1.9

4.1.10

4.1.11

4.1.12

4.1.13

4.1.14

4.1.15

## Wait 25-30 minute for the system to achieve steady state

4.1.16

Now take out the samples from the bottom & distillate stream (by closing
the timer for short while)

4.1.17

Cool down the samples to room temperature and measure the refractive
indices

4.1.18

indices

4.1.19

## Note down the temperature and refractive indices

4.1.20

Now adjust the cyclic timer to a desired reflux ration and for 3-5 min

4.1.21

Now takes out the samples from both distillate and bottom product

4.1.22

Cool down the samples to room temperature and measure the refractive
indices

4.1.23

indices

4.1.24

## Note down the temperature and refractive indices

4.1.25

Repeat the experiment for different set point temperatures and reflux
ratios

4.2

Closing Procedure:
4.2.1

4.2.2

4.2.3

## 5. Results and analysis

5.1
(a) Data
Relative volatility
Molecular weight of methanol MM
Molecular weight of Water MW
Enthalpy of feed HF
Packed height Z

3.32
32 g/mole
18 g/mole
0 kJ/kmole
0.90 m

(b)Observations
Total reflux condition

Time
T (OC)
R.I

5.2

Time
T (OC)
R.I

Calculations

## a) For total reflux condition

x _________ [From R.I vs x graph]

Time

T (OC)

## xF _________ [From R.I vs x graph, value of x corresponding to R.IF]

xB _________ [From R.I vs x graph, value of x corresponding to R.IB]
xD _________ [From R.I vs x graph, value of x corresponding to R.ID]
o

xthe

x

T(OC)

Time

y
Time

x
1 (
1)x

T(OC)

## To calculate the property of methanol (CPM ,M ) and water (CPW ,W ) at

temperature TB (oC) from data book.

6. Nomenclature:

7. Block diagram

## EXPERIMENT 2: SIEVE PLATE DISTILLATION COLUMN

1. Objective
To operate the column under total reflux condition and calculate the minimum number of
theoretical stages using fenskes equation. To operate the column under any desired
reflux condition and calculate theoretical number of stages using Mc-Cabe Thieles
method

2. Description
The set-up consists of column with seven sieve trays. A vessel is provided with funnel, at
the bottom of the column. A sight glass is provided with it and two other sight glasses is
given at middle of the column. Safety valve and pressure gauge are given at vessel. A
tank is provided to collect the bottom product. Shell and tube type condenser is provided
to condensate the vapour. Reflux drum is provided to collect the condensate. Receiving
tank is for collecting the distillate. Seven valves are provided at each plate for collecting
the samples. Drain valves are provided for drainage purpose. Temperature sensors are
fitted at the appropriate place to measure the temperatures.

3. Theory
4.1
Part 1
In sieve plate distillation column sieve plate are provided instead of packing material.
For simple batch distillation process, initially the still is filled with F moles of feed with
xF as the mole fraction of the more volatile component. Let at any moment the number
of moles of liquid in the still be B having a mole fraction x of the more volatile
component (A) and let the moles of accumulated condensate be D. Concentration of the
equilibrium vapour is y*. Over a small time, the change in the amount of liquid in the
still is dB and the amount of vapour withdrawn is dD. The following differential mass
balance equations may be written:

## The above equation is more convenient form of rayleigh equation.

Batch distillation with only a single still does not give a good separation unless the
relative volatility is very high. To obtain product with a narrow composition range, a
rectifying batch still is used that consist of a reboiler, a rectifying column, a condenser,
some means of splitting of a portion of condensed vapor or distillate as reflux and the
receiver. The operation of a batch still and column can be analyzed using the same
operating line equation as for the rectifying section of the continuous distillation:

Since the slope of the operating line is R / (R+1), the slope increases as the reflux
increases, until when reflux is infinite. Under total reflux slope is 1. The operating line
then coincides with the diagonal. The number of plate is minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of
xB and xD based on the relative volatility of the components , which is defined in terms
of equilibrium concentrations:
Minimum number of theoretical plates required:

## The above equation is known as fenskes eqn.

The final ratio does not change much over the range of temperature encountered in a
typical column, so the relative volatility is taken as constant.
4.2 Part 2: Method to calculate number of theoretical plates (Mc-Cabe Thieles
Method):
For the determination of number of theoretical plates at desired reflux ratio, we are using
graphical method which is called Mc-Cabe Thieles method. In this method draw the
equilibrium data on x-y plane. Locate the point xD, xB, and xF on diagonal. For the
given reflux ratio R calculate the intercept on the rectifying section operating line on the
y-axis.

## Where q is the fraction of liquid in the feed.

Follow the following procedure to calculate theoretical number of plates (Nt):
Plot the equilibrium data on x-y plane.
Locate the point xD, xB, and xF on diagonal.
Draw the rectifying line from point xD with intercept I on the y axis.
Also draw the feed line from the point xF with slope S and intersect the rectifying line,
that intersection point is M.
Now draw the stripping line from point xB to the intersection point M.

## Draw horizontal line from the point xD to equilibrium curve.

Draw vertical line from the point at equilibrium curve (where horizontal line is end) to
the operating line.
The above step made triangular construction.
Again draw horizontal line from the point at operating line (where vertical line is end) to
the equilibrium curve.
Repeat the above three steps between equilibrium curve and operating line, till cover the
point xB on diagonal.
Count the number of triangles made.
Number of triangles is equal to number of theoretical stages including reboiler.
Subtract one from the number of triangle, and then it is theoretical number of stages
required at desired reflux conditions.
For the overall efficiency of the column can be use following formulae:

4. Experimental Procedure
5.1 Starting Procedure
5.1.1 Measure the refractive index of feed solution.
5.1.2 Note down the volume of methanol.
5.1.3 Close all the valves V1-V13.
5.1.4 Ensure that ON/OFF switches given on the panel are at OFF position.
5.1.5 Fill vessel with methanol-water solution by open the funnel valve V 1 and
5.1.6
5.1.7
5.1.10

## air vent valve V2.

Close the funnel valve V1 and the air vent valve V2.
Switch ON the main power supply.
Set the temperature of solution above boiling point of methanol but less
than 100oC (say 90oC) by the DTC.

## 5.1.11 Switch ON the heater.

5.1.12 Switch ON the cyclic timer and set the total reflux condition.
5.1.13 Open the air vent valve V10 provided at the top of condenser and after
observing vapour coming out of it close the valve V10.
5.1.14 Switch ON the pump and set the condenser cooling water flow rate by
5.1.15
5.1.16
5.1.17
5.1.18

Wait till required temperature or steady state condition achieves.
Note down the temperatures of each tray.
Now take out the samples from each tray by open the valve V3-V9.
Also collect the distillate and bottom product by open the valve V11 and

V13 respectively.
5.1.19 Cool down the samples to room temperature & measure their refractive
indices.
5.1.20 Now adjust the cyclic timer to a desired reflux ratio & wait for steady
state.
5.1.21 Note down the temperatures of each tray.
5.1.22 Now take out the samples from each tray by open the valve V3-V9
5.1.23 Also collect the distillate and bottom product by open the valve V11 and
V13 respectively
5.1.24 Cool down the samples to room temperature & measure their refractive
indices.
5.1.25 Repeat the experiment for different set point temperatures & reflux ratios

5.2

Closing Procedure
5.2.1 When experiment is over switch OFF the heater.
5.2.2 Switch OFF the main power supply.
5.2.3

## Results and analysis

6.1
(a) Data
Relative volatility
Molecular weight of methanol MM
Molecular weight of Water MW
Enthalpy of feed HF
Packed height Z

3.32
32 g/mole
18 g/mole
0 kJ/kmole
0.90 m

(b)Observations
Total reflux condition

Time
T (OC)
R.I

6.2

Time
T (OC)
R.I

Calculations

## a) For total reflux condition

x _________ [From R.I vs x graph]

Time

T (OC)

## xF _________ [From R.I vs x graph, value of x corresponding to R.IF]

xB _________ [From R.I vs x graph, value of x corresponding to R.IB]
xD _________ [From R.I vs x graph, value of x corresponding to R.ID]
o

xthe

x

T(OC)

Time

y
Time

x
1 (
1)x

T(OC)

## To calculate the property of methanol (CPM ,M ) and water (CPW ,W ) at

temperature TB (oC) from data book.

Nomenclature:

7. Block diagram

## EXPERIMENT 3: STEAM DISTILLATION COLUMN

1. Objective
To calculate the percentage recovery of turpentine oil.

2. Description
The set-up consists of jacketed pressure vessel. Steam generator is provided to
generate the steam. Condenser is given to condensate the vapour. Rotameter is provided
to measure the flow rate of cooling water supply. Steam trap is for releasing the pressure.
Digital temperature indicator & digital temperature controller are provided to indicate
and control the temperature.
3. Procedure
4.1 Starting Procedure
4.1.1 Take known amount of turpentine oil and note down the volume of it.
4.1.2 Take known amount of water, note down the volume of it & mix it with
turpentine oil.
4.1.3

## Close all the valves V1-V11.

4.1.4

Ensure that ON/OFF switches given on the panel are at OFF position.

4.1.5

Fill water in the steam generator by open the valve V1 and air vent valve
V2 and close them.

4.1.6

Charge the distillation still with turpentine oil & water mixture by open

4.1.7
4.1.8

## the valve V6 and air vent valve V7.

Switch ON the main power supply.
Set the temperature of steam generator with the help of DTC (approx.

4.1.9
4.1.10
4.1.11
4.1.12

115C).
Switch ON the heater.
Wait for the steam formation.
As steam formed, open the steam supply valve V3.
Start the supply of steam in jacket by open the valve V 4 and air vent valve

V9.
4.1.13 When the temperature in the still reaches 2C below the distillation
4.1.14
4.1.15
4.1.16
4.1.17

temperature, stop the supply of steam in jacket by close the valve V4.
Start the flow of live steam by open the valve V5.
Connect cold water supply to condenser.
Note down the live steam pressure.
Collect the condensed vapors in glass separating chamber.

4.1.18
4.1.19
4.1.20
4.1.21

## Continue the distillation process for sufficient time (approx 1 hr).

Stop the steam supply and collect the distillate in separate chamber.
Wait for the formation of two layers.
Collect the separate formed layers by open the valve V8 & weigh them.

## 4.2 Closing Procedure

4.2.1 When experiment is over stop the water supply.
4.2.2 Switch OFF the heater.
4.2.3 Switch OFF the main power supply.
4.2.4 Drain the vessel by open the valve V10.
5

## Results and Analysis

5.1 (a) Data
Molecular weight of turpentine oil MA = 136 g/mole
Molecular weight of water MB = 18 g/mole
(b) Observations:
Po

= __________ kg/cm2
T = __________oC

VA

= __________ Lit.

VB

= __________ Lit.

= __________ Lit.

5.2 Calculations
To calculate the property of turpentine oil ( A ) and water ( B ) at temperature T
(oC) from data book.
A = ________ (kg/m3)
= ________ (kg/m3)

from data book.
A

= 13.84799

= 3377.754
C

= 62.817

6. Nomenclature

7. Block Diagram

## EXPERIMENT 4: VAPOUR IN AIR DIFFUSION APPARATUS

1. OBJECTIVE:
To determine the diffusion coefficient of an organic vapor in air.
2. DESCRIPTION:
The equipment consists of a T tube made of glass, placed in a water bath. Water bath
is provided with heater. Temperature of the bath is controlled by the digital
temperature controller. Stirrer is given to maintain the constant temperature in bath.
Air pump is provided to supply the air, passed through the tube. Change in the liquid
level is observed by the traveling microscope with sliding vernier scale.
3. EXPERIMENTAL PROCEDURE:
4.1.STARTING PROCEDURE:
4.1.1. Clean the apparatus and make it free from dust.
4.1.2. Ensure that switches given on the panel are at OFF position.
4.1.3. Fill the water bath with water 3/4th of its capacity.
4.1.4

4.1.5

4.1.6

4.1.7

## Switch ON the stirrer.

4.1.8

Wait till the bath attains the set temperature. Note the steady temperature
of the bath.

4.1.9

capillary leg.

## 4.1.10 Note down the initial height of liquid in the capillary.

4.1.11 Make the connection with air pump and allow a gentle current of air to
flow over the capillary.
4.1.12 Record the height of liquid in the capillary after every 10 min. .
4.1.13 Repeat the experiment for different water bath temperatures.

4.2.1

4.2.2

4.2.3

4.2.4

5.1 Data

5.2 Observation
T = _________ C
X= _________ cm
No.

5.3 Calculations

t(min)

X(cm)

No.

6. Nomenclature

t1(sec)

x(cm)

7. Block Diagram

## EXPERIMENT 5: MASS TRASNFER WITH & WITHOUT CHEMICAL REACTION

(SOLID LIQUID SYSTEM)

1. Objective
To study the dissolution of benzoic acid in water and in aqueous solution of sodium
hydroxide.
2. Aim
2.1 To calculate the mass transfer coefficient (kr) with chemical reaction.
2.2 To calculate the mass transfer coefficient (k) without chemical reaction.
2.3 To calculate the experimental enhancement factor (exp ) for the given system.
2.4 To calculate the theoretical enhancement factor (THE ) for the given system by
film and boundary layer model.
3. Description
The set up consists of a reactor with stirrer, connected with a variable speed mixer.
Baffles are provided in the mixer. RPM sensor is given to sense the speed of stirrer. A
peltilizer is provided to make the solid cylinder of benzoic acid. Constant temperature
water bath arrangement is provided with heater to conduct the experiment at various
temperatures. Valves are provided for drainage purpose.
4. Procedure
4.1 Starting procedure (for mass transfer with chemical reaction)
4.1.1 Prepare the benzoic acid cylinder first by using the peltilizer.
4.1.2 Record the dimensions of the benzoic acid cylinder.
4.1.3 Fill the burette with N/50 HCl solution.
4.1.4 Ensure that switches given on the panel are at OFF position.
4.1.5 Close all the valves V1-V2.
4.1.6 Fill the water bath with water.
4.1.7 Set the desired temperature of water bath (ambient to 50 oC).
4.1.8 Fill the reactor with aqueous sodium hydroxide solution of known
concentration up to 2/3rd of its volume.
4.1.9

## 4.1.10 Switch ON the main power supply to the set-up.

4.1.11 Switch ON the heater.
4.1.12 Wait till the aqueous solution attains the desired temperature.
4.1.13 Note down the temperature.
4.1.14 Now fix the benzoic acid cylinder inside the reactor containing aqueous

## sodium hydroxide solution.

4.1.15 Switch ON the motor and stirrer and fix the RPM of it. Take 10 mL
sodium hydroxide solution inside the reactor for initial reading of titration.
Titrate

the

sample

solution

against

N/50

HCl

solution

using

## phenolphthalein as an indicator (Add HCl from burette). Note down the

volume of N/50 HCl used in titration.
4.1.16 Take the sodium hydroxide sample for titration at every interval time until
the reading become constant. Titrate the sample solution against N/50 HCl
solution using phenolphthalein as an indicator (Add HCl from burette).
Note down the volume of N/50 HCl used in titration.
4.1.17 Stop the motor and remove the benzoic acid cylinder.
4.1.18 Measure the benzoic acid cylinder dimensions again.
4.2 Starting procedure (for mass transfer without chemical reaction)
4.2.1 Prepare the benzoic acid cylinder first by using the pertilizer.
4.2.2 Record the dimensions of the benzoic acid cylinder.
4.2.3 Fill the burette with N/20 NaOH solution.
4.2.4 Ensure that switches given on the panel are at OFF position.
4.2.5 Close all the valves V1-V2.
4.2.6 Set the desired temperature of water bath (ambient to 50oC).
4.2.7 Fill the reactor with de-ionized water up to 2/3rd of its volume.
4.2.8 Note down the volume of de-ionized water.
4.2.9

## 4.2.10 Switch ON the heater.

4.2.11 Wait till the water attains the desired temperature.
4.2.12 Note down the temperature.
4.2.13 Now fix the benzoic acid cylinder inside the reactor containing deionized water.
4.2.14 Switch ON the motor and stirrer and fix the RPM of it. Take 10 mL of
water inside the reactor for initial reading of titration. Titrate the sample
solution against N/20 NaOH solution using phenolphthalein as an
indicator (Add NaOH from burette). Note down the volume of N/20
NaOH used in titration.
4.2.15 Take the sodium hydroxide sample for titration at every interval time until
the reading become constant. Titrate the sample solution against N/20
NaOH solution using phenolphthalein as an indicator (Add NaOH from
burette). Note down the volume of N/20 NaOH used in titration.
4.2.16 Stop the motor and remove the benzoic acid cylinder.
4.2.17 Measure the benzoic acid cylinder dimensions again.

4.3.1

4.3.2

4.3.3

4.3.4

4.3.5

## 5. Result & Analysis

5.1 (a) Data
Solubility of benzoic acid in NaOH with reaction CR*
Solubility of benzoic acid in water without reaction C*
Rod diameter drod
Diffusivity of NaOH DA
Diffusivity of benzoic acid DB
Initial concentration of benzoic acid in liquid Bo
Number of moles of NaOH taking part in the chemical
reaction nB

## (b) Observation (for with chemical reaction)

T

= ____________ oC

Di

= ____________ m

Df

= ____________ m

Li

= ____________ m

Lf

= ____________ m
N = ____________ RPM

N1w
V2

= ____________ g eq/L
= ____________ ml

V = ____________ Lit

= 0.0276 kmole/m3
= 0.00321 kmole/m3
= 0.006 m
= 1.04 x 10-9 m2/sec
= 4.1 x 10-9 m2/sec
= 0.5
=1

No.

t (sec)

V1W (ml)

## (c) Observation (for without chemical reaction)

T

= ____________ oC

Di

= ____________ m

Df

= ____________ m

Li

= ____________ m

Lf

= ____________ m
N = ____________ RPM

N1

= ____________ g eq/L

V2

= ____________ ml
V = ____________ Lit

Sr. No.

5.2

t (sec)

V1 (ml)

Sr. No.

t (sec)

CW (kmole/m3)

1-

CW
C

ln 1

CW
C

6. Nomenclature

7. Block diagram

## EXPERIMENT 6: FLUIDIZED BED DRYER

1. Objective
To plot the drying curve under fluidized bed condition.
2. Description
The set up consists of a vertical glass column. The lower portion of the column is filled
with fluidizing material. The material is supported on the screen mesh held between
two flanges. Air is supplied through a blower in heater box. Orifice with differential
manometer is provided to measure the air flow rate. Flow control valve and by-pass
valve are given to regulate the airflow. A cyclone is provided at the top outlet of the
column to collect solid particle taken out by the air stream. Sensors are given at
different positions to measure the temperature.
3. Procedure

3.1

Starting procedure
3.1.1

3.1.2

3.1.3

3.1.4

3.1.5

## Connect the electric supply to the set-up.

3.1.6

Start the blower and adjust the air flow rate by open the valve V1.
3.1.7

3.1.8

## increment or decrement and set button of DTC.

Allow the air to pass through the bypass line valve. Start the
heater and wait till desired temperature of air is reached.

3.1.9

Open the lid of column fill the conical portion of the dryer with
the wet material and close the lid.

3.1.10 Allow the hot air at prefixed flow rate and temperature to pass
through the dryer.
3.1.11 The flow rate should be sufficient to fluidize the material.
3.1.12 At regular intervals of time take out measurable amount of wet
material and weigh it.
3.1.13 Dry it completely and weigh it again.
3.2

Closing procedure
3.2.1

3.2.2

## 4. Results & Analysis

4.1 (a) Data
Diameter of orifice do
Diameter of pipe dp
Coefficient of discharge Cd
Acceleration due to gravity g
Density of water w
Density of air a
Molecular weight of water MW
Molecular weight of air MA
(b) Observations
W = ________ gm

= 0.026 m
= 0.052 m
= 0.6
= 9.81 m/sec2
= 1000 kg/m3
=1.21 kg/m3
= 18 g/mole
= 29 g/mole

Z = ________ gm

No.

4.2

t (sec)

WD (gm)

h1 (cm)

## h2 (cm) TW1 (C)

Calculations

Experimental Calculation:
Z
C W
(kg water/kg dry solid) (at t =0)
O
W

C Z WD
WD

## Td1 (C) TW2 (C)

TW1 (C)

W W D
C=
(kg water /kg dry solid )
WD

x=

Co C
( kg water /kg dry solid )
Co C

Calculation Table: 1
Sr. No.
X (kg water/kg dry solid)

t(sec)

S=

dx
dt

## N exp dx (Kg water/Kg dry solid-sec)

dt
Theoratical Calculation:

To calculate the humidity (y1 & y2) of air at temperature (Tw1 & Td1) and (Tw2 & Td2)
respectively by psychometric chart.

Calculation Table: 2

Sr. No.

5. Nomenclature

t (sec)

6. Block Diagram

## EXPERIMENT 7: ADSORPTION IN PACKED BED

1. Objective
To calculate the length of unused bed for the given system.
2. Description
The set-up consists of three borosilicate columns having different diameters & lengths.
For flow of fluid a pump & rotameter is provided. At the inlet of column, valves are
provided to feed only one column at a time. Valves are provided at the bottom of
columns & liquid tanks to drain out after running the apparatus. Filters are provided
before the column drain valves to prevent the charcoal from drain.
3. Procedure
4.1 Starting procedure
4.1.1 Prepare 20 liter of colored liquid by dissolving known amount of KMnO4 in
4.1.2
4.1.3
4.1.4
4.1.5
4.1.6
4.1.7
4.1.8
4.1.9
4.1.10
4.1.11
4.1.12
4.1.13

20 liter of water.
Close all the valves V1-V10.
Ensure that switches given on the panel are at OFF position.
Fill colored liquid in the feed tank.
Keep activated charcoal in all the columns.
Connect electric supply to the set-up.
Open the valve V3 of the column-1.
Partially open the by pass valve V2.
Switch ON the pump.
Open and adjust the flow control valve V1 and by pass valve V2.
Simultaneously start the stop watch.
Collect samples from out let of column-1 after a time intervals.
Note down the time.

4.1.14

## Measure the optical densities of the samples.

4.1.15

Run the experiment till the change in color of outlet liquid becomes almost
stable.

4.1.16

4.1.17

4.1.18

4.1.19

4.1.20

4.1.21

## Measure the optical densities of the samples.

4.1.22

Run the experiment till the change in color of outlet liquid becomes almost

stable.

4.1.23

4.1.24

4.1.25

4.1.26

4.1.27

4.1.28

## Measure the optical densities of the samples.

4.1.29

Run the experiment till the change in color of outlet liquid becomes almost

stable.
4.1.30

## 4.1 Closing procedure

7.2.1
When experiment is over stop the supply of feed by close the valve V1.
7.2.2
Switch OFF the pump.
7.2.3
Switch OFF the main power supply.
7.2.4
Drain the columns by open the valve V6, V7 and V8.
7.2.5

7.2.6

## Drain the product tank by open the valve V10.

7.2.7

Remove the charcoal by open the filter cups of the columns properly.

## 5 Results & Analysis

5.1 (a) Data
Length of column L1
Length of column L2
Length of column L3

=1m
= 0.5 m
= 0.3 m

(b) Observations
F = ________ LPH
O.D.F = ________

Sr. No.

(min)

O.D

5.2 Calculations
CF =________[From O.D. vs C graph value of C corresponding to O.D. F]
C = ________ [From O.D. vs C graph value of C corresponding to O.D.]

Sr. No.

(min)

## Plot the graph of (C/CF) vs and find out S, B.

O.D

C/CF

S = ________ (min)[From the graph, time at which areas of the shaded portions are equal]
B = ________ (min)[From the graph, time at which initial minimum concentration shows]

Nomenclature