Mto Lab Manuals - All Experiments

JAYPEE UNIVERSITY OF ENGINEERING & TECHNOLOGY, GUNA
Department of Chemical Engineering

List of Experiments in Mass Transfer Operations
Laboratory
1. LIQUID-LIQUID EXTRACTION IN A PACKED BED COLUMN
2. ADSORPTION IN PACKED BED COLUMN
3. PERFORMANCE OF WATER COOLING TOWER
4. WETTED WALL COLUMN
5. DIFFUSION COEFFICIENT OF ACETONE (VAPOR) IN AIR
6. GAS ABSORPTION IN MECHANICAL AGITATOR
7. BATCH CRYSTALLIZATION
8. DIFFERENTIAL DISTILLATION
9. ABSORPTION IN PACKED BED COLUMN
10. BATCH RECTIFICATION IN PACKED BED COLUMN
11. BATCH RECTIFICATION IN A SIEVE PLATE COLUMN
12. TO DETERMINE THE DIFFUSIVITY COEFFICIENT BY PITOT TUBE
13. STEAM DISTILLATION
14. ROTARY DRYER
15. FORCED DRAFT TRAY DRYER
16. HUMIDIFICATION-DEHUMIDIFICATION COLUMN
17. LIQUID-LIQUID EXTRACTION IN A SPRAY COLUMN
18. SOLID-LIQUID EXTRACTION UNIT (BONNOTTO TYPE)
19. FLUIDIZED BED DRYER
MASS TRANSFER OPERATIONS LAB
1
Experiment No: 01
LIQUID-LIQUID EXTRACTION IN
A PACKED BED COLUMN
2
LIQUID-LIQUID EXTRACTION IN A PACKED BED COLUMN
OBJECTIVE:
To study the extraction of benzoic acid from mixture of toluene and benzoic acid (dispersed phase) by
water (continuous phase) in a packed bed.
AIM:
1. To determine overall mass transfer coefficient based on continuous phase (water), K
w
a
2. To determine overall mass transfer coefficient based on dispersed phase (toluene), K
t
a
3. To determine overall Height of Transfer Unit based on continuous phase (water), HTU
ow
4. To determine Individual Height of Transfer Unit based on continuous phase (water), HTU
w
and
dispersed phase (toluene), HTU
t
INTRODUCTION:
Liquid extraction sometimes called solvent extraction is the separation of the constituents of a liquid
solution by contacting with another insoluble liquid. If the substances constituting the original solution
distribute themselves differently between the two liquid phases, a certain degree of separation will result
& this can be enhanced by the use of multiple contacts or their equivalent in the manner of gas
absorption and distillation.
THEORY:
Towers filled with some random packing (say raschig rings) are widely used for extraction of valuable
chemicals from dilute solutions by liquid-liquid extraction. The packing provides a larger extraction area
for mass transfer and also reduces the axial mixing to some extent. The extraction rate in such columns
depends on:
(a) Choice of either continuous or dispersed phase.
(b) Packing and column variables.
(c) Velocity of liquid phases in the tower.
The tower performance is generally based on extraction rate data and evaluated in terms of overall height
of transfer unit, based on continuous phase, HTU
ow
and the extraction factor expressed in terms of flow
rate ratios of the liquid phase,
t
w
V
mV
. These two variables are plotted against each other on Cartesian co-
ordinates. As suggested by Colburn, the slope and intercept of such a plot would represent the resistance
of the individual films as:
OVERALL HEIGHT OF TRANSFER UNIT:
HTU
ow
= HTU
w
+ HTU
t
[mV
w
/V
t
]
HTU
ot
= HTU
t
+ HTU
w
[V
t
/mV
w
]
Where m is the slope of equilibrium curve, m= dC
w
/dC
t
Under equilibrium conditions (e.g. low concentrations) m is a constant.
3
V is the superficial velocity of the liquid phase based on empty cross section of the column, subscript
w for continuous phase (water) and t for dispersed phase (toluene). Rate of mass transfer from
dispersed phase to continuous phase is defined as:
( ) ( )
( ) ( ) [ ]
1
]
1

2 2 1 1
2 2 1 1
/ ln
w w w w
w w w w
w
C C C C
C C C C
aV K
N
(1)
or
( )
1
]
1
2 1
2 1
/ ln C C
C C
aV K
N
w
(2)
the capacity coefficient based on continuous phase (water), K
w
a, is thus defined as:
( )
ln w
w
C V
N
a K
(3)
where,
( )
,
_

2
1
2
ln
ln
w
w
w w
w
C
C
C C
C
Similarly, the capacity coefficient based on dispersed phase (toluene), K
t
a, is defined as:
( )
ln t
t
C V
N
a K
(4)
As per Chilton and Colburn, the overall height of transfer unit based on continuous phase (water),
HTU
ow
is defined as:
a K
V
HTU
w
w
ow

(5)
and the overall height of transfer unit based on dispersed phase (toluene), HTU
o
t is defined as:
a K
V
HTU
t
t
ot

(6)
DESCRIPTION:

In this system two different liquids are used in which the one is heavier (water) which is used as solvent
and other is lighter in which the solute is present (toluene). The heavier liquid is inserted from top and
lighter from the bottom. The interface maintained in the column between the lighter phase and the
heavier phase at the top of the column can be adjusted up or down as necessary by regulating the
arrangement provided at the water stream leaving the column. The position of the interface to be
4
maintained at about 1 inch above the point of introduction of the heavier liquid (water in this
case) into the column. The samples are taken from the top for lighter liquid and bottom for heavier liquid
and are analyzed.
UTILITIES REQUIRED:
1. Compressed Air Supply at 2 Bar, 0.5 CFM
2. Drain
3. Laboratory Glassware
4. Water Supply
5. Weighing Balance (least count 1gm)
CHEMICALS REQUIRED:
1. Toluene = 20 Ltrs
2. Benzoic Acid = 500gms
3. Distilled Water = 20 Ltrs
4. N/5 NaOH in alcohol = 500ml
5. N/20 NaOH in water = 500ml
6. Phenolphthalein as indicator = 10ml
EXPERIMENTAL PROCEDURE:
For the case where continuous phase (water) flow is downwards while the dispersed phase (Toluene +
Benzoic Acid) flow is upwards, the extract will be collected through the bottom while the raffinate will
be collected from the top.
1. Prepare a mixture of toluene and benzoic acid as a feed mixture, with the concentration of benzoic
acid in the range of 0.1- 0.2 kmol/m
3
means 24.4gm/lit or 488gm in 20litres (i.e N/5)
2. Fill the column with the continuous phase (water).
3. Allow the dispersed phase (toluene+ benzoic acid) to enter from the bottom of the column at some
minimum rate.
4. Adjust the rotameter readings for both the phases (1 to 5 LPH for dispersed phase and 3 to 10 LPH
for continuous phase).
5. The interface between the lighter phase and the heavier phase at the top of the column must be
worked up or down as necessary by regulating the valve in the water stream leaving the column. The
position of the interface is to be maintained at about 1 inch above the point of introduction of the
heavier liquid.(water) into the column.
6. In case lighter liquid is the continuous phase, the same arrangement should be used to maintain the
interface.
7. Take the first observation after the steady state has been established i.e after 10 to 20 minutes.
8. Collect the samples of extract and raffinate and measure the concentration of benzoic acid in each by
titrating a known volume of sample with standard NaOH solution using phenolphthalein as indicator.
Use standard NaOH solution in alcohol (N/5) for titration against toluene and NaOH solution ( N/20)
in water for titration against water.
9. Repeat the above steps for 5 to 6 different flow rates of continuous/dispersed phase.
5
SPECIFICATION:
Extraction Column : Material Borosilicate Glass
Dia. 45mm, Height 750mm (approx)
Packing Material : Borosilicate Glass Raschig Rings Size 8-10mm (approx.)
Feed Tanks : Material SS, Capacity 20 Ltrs, 2 No.s
Extract and Raffinate Tanks : Material SS, Capacity 10 Ltrs, 2 No.s
Piping : SS and PVC, Size
Feed Circulation : By compressed air
Pressure Regulator : 0-2 kg/cm
2
Pressure Gauge : Bourdan type, 0-2 kg/cm
2
Flow Measurement : Rotamaters (One each for Continuous phase and dispersed phase)
Special arrangement for changing interface zone at any level in extraction column.
OBSERVATION & CALCULATION:
DATA:
Column Diameter, Dc = 40mm
Packed height, Z = 750mm
Column cross sectional area =
2 2
4
m D
c
Effective volume,V = ) (
4
3 2
m z D
c
Packing = Raschig rings

Diameter of Raschig ring = 9mm
Length of raschig ring = 10mm
Ambient temperature = T, C
System : Toluene-Benzoic Acid-Water
Solute : Benzoic Acid
Initial conc. of benzoic acid in Toluene, C
T1
= gmol/L
Initial conc. of benzoic acid in Water, C
w2
= 0.0 gmol/L (Using pure water)
Benzoic Acid: Molecular Formula = C
7
H
6
O
2
Molecular mass = 122
Equivalent wt. = 122
Toluene: Molecular formula = C
7
H
8
Molecular mass = 92
Equivalent wt. = 92
6
OBSERVATION TABLE:

S.No. Flow rate of
toluene phase,
Q
t
in L/h
Flow rate of water
phase, Q
w
in L/h
Volume of N/5
NaOH(in alcohol)
used for titration for
10ml of toluene
solution
Volume of N/20
NaOH(in water)
used for titration for
10ml of water
solution
CALCULATION:
A) CONCENTRATION OF BENZOIC ACID IN TOLUENE:
1) At bottom : (feed concentration)
Volume of sample ( Toluene feed solution) V
1
= ml
Normality of sample N
1
= ?
Normality of NaOH (in alcohol) used V
2
= ml
Normality of NaOH (in alcohol) used N
2
= 1/5
2 2 1 1
N V N V

1
2 2
1
V
V N
N
Conc. of Benzoic Acid in the Toluene at bottom, C

T1
= N
1
gmole/L
2) Similarly at the top:

1
2 2
1
V
V N
N
Conc. of benzoic acid in toluene at top, C
T2
= gmole/L
Volumetric flow rate of Toluene Phase Q
T
= LPH

Amount of Benzoic acid extracted by water A

1
= (C
T1
-C
T2
)Q
T
gmole/h
B) CONCENTRATION OF BENZOIC ACID IN TOLUENE:
1) Top : Pure water C
w2
= 0
2) Bottom:
Volume of water sample used for titration = V
1
ml
Normality of acid in water = N
1
Volume of NaOH used for titration = V
2
ml
Normality of NaOH used for titration = N
2

1
2 2
1
V
V N
N
gm eq/L
Concentration of acid in water at bottom = C
w1
g mole/L
Volumetric flow rate of water = Q
w
LPH
7

Amount of Benzoic acid recovered by water A

2
= (C
w1
-C
w2
)Q
w
g mole/h
Average amount of Benzoic Acid recovered,

2
2 1
A A
N
+
gmole/h
OVERALL MASS TRANSFER COEFFICIENT ON DISPERSED PHASE:
(K
t
a)
At bottom:
C
T1
= g mole/L
C
w1
= g mole/L
H
1
=
1 T T
C atC
t
w
C
C
1
]
1
(using the equilibrium data)

C
T1
= C
T1
- (C
W1
/H
1
) g mole/L
At Top:
C
T2
= g mole/L
C
w2
= 0
H
2
=
T
w
C
C
at C
T
= C
T2
C
T2
= C
T2
- (C
W2
/H
2
) g mole/L
( )
( )
1 2
1 2
ln
/ ln
T T
T T
T
C C
C C
C

(C
T
)
ln
= g mole/L
Since N/ = K
t
a V (C
T
)
ln
K
t
a =
( )
ln T
C V
N
(g mol/ h-L-gmol/L)
1 1 1 1 w T w
C C H C
2 2 2 2 w T w
C C H C
( )
1
2
1 2
ln
ln
w
w
w w
w
C
C
C C
C

g mol/L
( )
ln
/
w
w
C V
N
a K

g mol/L-h-C
Overall height of transfer unit based on continuous phase:
Superficial velocity of water phase, V
w
= Q
w
/A
c
m/hr
HTU
ow
=
a K
V
w
w
m
8
Overall height of transfer unit based on dispersed phase:
Superficial velocity of toluene phase, V
t
= Q
t
/A
c
m/hr
HTU
OT
=
a K
V
t
t
m
Repeat the above calculations for five different flow rate ratios of continuous and dispersed phase
(V
w
/V
t
) and use equations (1 and 2) to determine the individual Height of Transfer unit based on
continuous phase (HTU)
w
and Height of Transfer Unit based on dispersed phase (HTU)
t
, by plotting
(HTU)
ow
vs
t
w
V
V
on a simple graph. Determine the slope and
intercept.
Intercept = (HTU)
w
Slope = (HTU)
t
Slope
Intercept
CALCULATION TABLE:
Run
No.
(HTU)
ow
m (HTU)
oT
m
m
t
w
V
V
w
t
mV
V (HTU)
w
m (HTU)
T
m
Equilibrium data for Benzoic Acid-Toluene-Water
Aqueous Phase, C
w
g mole/L, Benzoic Acid Organic Phase, C
T
g mole/L, Benzoic Acid
0.0000 0.0000
0.0016 0.0080
0.0064 0.0336
0.0080 0.0673
0.00961 0.08811
0.011211 0.12015
9
Run
No.
C
w1
gmol/L C
w2
gmol/L C
T1
gmol/L C
T2
gmol/L Rate of M.T,
N/ gmole/h
0.012816 0.14097
0.01442 0.17301
The equilibrium data can be represented by;
2
3672 . 4 4273 . 1 2015 . 0
T T
T
w
C C H
C
C
+
and
0019 . 0 0745 . 0 +
T w
C C
or slope of the equilibrium line can be assumed to be constant at
0745 . 0
T
w
dC
dC
m
NOMENCLATURE:
C
w1
= concentration of benzoic acid in water at its outlet, kgmol/l
C
w2
= concentration of benzoic acid in water at its inlet, kgmol/l
C
T1
= concentration of benzoic acid in toluene at its inlet, kgmol/l
C
T2
= concentration of benzoic acid in toluene at its outlet, kgmol/l
C*
w
= equilibrium solute (benzoic acid) concentration in water phase
C*
T
= equilibrium solute (benzoic acid) concentration in toluene phase
H = Equilibrium distribution Coefficient (C*
w
/ C*
T
)
K
w
a = Overall mass transfer coefficient based on continuous phase
K
t
a = Overall mass transfer coefficient based on dispersed phase
N/ = kg mole of benzoic acid transferred from toluene to water per hour
Q
T
= flow rate of toluene, LPH
Q
W
= flow rate of water, LPH
V = is the effective volume of packed section, m
3
V
t
= toluene flow rate LPH/m
2
cross section of column
V
w
= water flow rate LPH/m
2
cross section of column
PRECAUTIONS AND MAINTAINENCE INSTRUCTIONS;
1. Interface should not be disturbed during the experiment.
2. Dont exceed the flow rate beyond 15LPH
3. Always use clean water & ensure that there are no foreign particles in it.
4. Always clean the column feed tanks & collecting tanks properly after experiment is over.
5. Never use feed tanks to store the chemicals used in the experiment.
10
6. Always drain the column once before running the experiment on desired second flow
rates.
==== X ====
11
Experiment No: 02
ADSORPTION IN PACKED BED
COLUMN
12
ADSORPTION IN PACKED BED
OBJECTIVE:
Study of Adsorption in a packed bed for a Solid Liquid System.
AIM:
Plotting the break through curve of adsorption for a given system and calculation of length of unused
bed for the system.
INTRODUCTION:
A substantial number of unit operations of chemical engineering are concerned with the problem of
changing the compositions of solutions & mixtures through methods not necessarily involving chemical
reactions. One of the well known operations for solid liquid contacting is adsorption. The colored
material which contaminates impure cane sugar solution can be removed by contacting the liquid
solutions with activated carbon, whereupon the colored substances are retained on the surface of the
solid carbon.
In adsorption the molecules distribute themselves between two phases, one of which is a solid whilst the
other can be the liquid or gas. Adsorption suffers one drawback, that the capacity of the adsorbent for the
adsorbate in question is limited. At intervals, the adsorbent has to be removed from the process and
regenerated, that is restored to its original condition. For this reason, in its early applications in industry,
the adsorption unit was considered to be more difficult to integrate with a continuous process.
THEORY:
Adsorption is the selective transfer of a solute from
a fluid phase to a batch of rigid particles. The usual
selectivity of a sorbent between solute and carrier
fluid or between different solutes makes it possible
to separate certain solutes from the carrier or from
one another.
It occurs when molecules diffusing in the fluid
phase are held for a period of time by forces
emanating from an adjacent surface. The surface
represents a gross discontinuity in the structure of
the solid and atoms at the surface have a residue of
molecular forces which are not satisfied by
surrounding atoms like those in the body of the
structure. These residual or Vander Waals forces
are common to all surface and the only reason that
certain solids are designated adsorbents is that
they can be manufactured in a highly porous form,
giving rise to a large internal surface.
Feed (a) (b) (c) (d)
Solution
Concen- Co Co Co Co
tration.
Adsorpti
on
Zone
Ads
Zone
Effluent
Concen- Ca Cb Cc Cd
tration
Break
through
Curve
0 Ca Cb Cc o Break Point
Volume of Effluent
13
The Adsorption Wave
The Adsorption Wave:
Consider a binary solution, containing a strongly adsorbed solute at concentration C
0
. The fluid is to be
passed continuously downwards through a relatively deep bed of adsorbent initially free of adsorbate.
The uppermost layer of solid, in contact with the strong solution entering, at first adsorbs solute is left in
the solution is substantially all removed by the layers of solid in the upper part of the bed. The effluent
from the top of the bed is practically solute-free, as at C
a
in the lower part of adjacent figure. The
distribution of adsorbate in the solid bed is indicated in the sketch in the upper part of this figure at (a),
where the relative density of the horizontal lines in the bed is meant to indicate the relative concentration
of adsorbate.
The uppermost layer of the bed is practically saturated, and the bulk of the adsorption takes place over a
relatively narrow adsorption zone in which the concentration changes rapidly, as shown. As solution
continues to flow, the adsorption zone moves downward as a wave, at a rate ordinarily very much slower
than the linear velocity of the fluid through the bed. At a later time, as at b in the figure, roughly half the
bed is saturated with solute, but the effluent concentration C
B
is still substantially zero. At c in the figure
the lower portion of the adsorption zone has just reached the bottom of the bed, and the concentration of
solute in the effluent has suddenly risen to an appreciable value C
C
for the first time. The system is said
to have reached the Breakpoint. The solute concentration in the effluent now rises rapidly as the
adsorption zone passes through the bottom of the bed and at d has substantially reached the initial
value c
o
. The portion of the effluent concentration curve between positions c andd is termed the
Breakthrough curve. If solution continues to flow, little additional adsorption takes place since the bed is
for all practical purposes entirely in equilibrium with the feed solution.
Length of Unused Bed Calculation:
Consider the adjacent figure. If the mass-transfer
rate were infinitely rapid, the breakthrough curve
would be the vertical line at
S
, which can be
located so that the shaded areas are equal. The
adsorption zone of the figure can then be idealized
as reduced to a plane, with the length of bed Z
S
upstream of the plane at concentration X
T
and the
length Z-Z
S
downstream equal to the length of
unused bed (LUB). At breakthrough, the length of
the bed is taken to be the sum of LUB and a length
saturated with solute in equilibrium with the feed
stream.
If V=velocity of advancement of the adsorption
plane, then at any time ,
Z = V,
at time
S
,
Z= V
S
, and at breakthrough,
Z
S
= V
B
; therefore:
LUB = Z-Z
S
= V(
S
-
B
) = Z (
S
-
B
) /
S
(1)
Y
0
Idealized

Y
0
True break through
Y
0
o

B

S
r

= time of effluent flow
14
DESCRIPTION:
The apparatus is provided for the process of Adsorption in Packed column with Solid phase being static
& fluid phase is following. For flow of fluid a pump & rotameter is provided. Three borosilicate
columns are provided having different diameters & lengths. 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.
UTILITIES REQUIRED:
Drain
Electricity Supply : 1 Phase, 220Volt AC and 1 KW
Floor Area : 1.2 m x 1m
Colorimeter or Spectrophotometer.
CHEMICALS REQUIRED:
Activated Charcoal : 1 Kg
KMnO
4
: 15 gms.
1. Check that all the valves are properly closed.
2. Fill the colored liquid in the feed tank (upper tank) and Activated Charcoal in columns.
3. The colored solution made; should not be too concentrated.
4. Open the valve of column to be operated.
5. Start the pump and the stop watch.
6. Fix a minimum flow rate using Rotameter.
7. Take the samples of the output from column after fixed time intervals.
8. Measure the Optical Density and hence concentration of color in the liquid.
9. Note down flow rate, time & concentration.
10. Run the fluid till the change in color of output liquid becomes almost stable.
11. Close the pump & valve of the column.
12. Now run for second & third columns.
SPECIFICATION:

Borosilicate Glass Column (3 nos.) : 1. Diameter = 30 mm, Length = 1000 mm
2. Diameter = 45 mm, Length = 500 mm
3. Diameter = 55 mm, Length = 300 mm
Liquid Flow Measurement : Rotameter (4 to 40 LPH)
Liquid Tank (2 nos.) : One each for Input and Output,
Material : Stainless Steel (SS)
Liquid Circulation : Magnetic Pump made of Polypropylene to Circulate Liquid phase.
Maximum working temperature is 85
0
C.
15
FORMULAE:
LUB = Z-Z
S
= V(
S
-
B
) = Z (
S
-
B
) /
S
V = Z /
S

OBSERVATION & CALCULATIONS:
A calibration curve between Optical Density & Concentration is plotted, as shown below.

O. D. vs Concentration (low concentration)
1E -06
8E -07 y = 2E 06 x
6E -07
4E -07
2E -07
0E +00

0 0.1 0.2 0.3 0.4 0.5
O.D.

Optical Density vs Concentration (high concentration)
1.2E -05
1.0E -05 y = 3E 06x
2
5E -07x + 6E - 07
8.0E -06
6.0E -06
4.0E -06
2.0E -06
0.0E +00

0.0 0.5 1.0 1.5 2.0
O.D.
16
Data :
Initial Optical density = I
0
Initial Concentration = C
0
(Using calibration chart)
Height of Charcoal in 1
st
column = Z
1

nd
column = Z
2

rd
column = Z
3

OBSERVATION TABLE :
Flow rate = F LPH
Height of bed in first column = Z
m

Time - Optical Density of Product - I
Wt. of product collected - W
CALCULATIONS:
A curve between & C
is plotted, which is called Breakthrough Curve. A curve between W

& C
may
also be plotted. Z
S
is calculated using flow rate V and saturation time
B
. Then length of unused bed is Z-
Z
S
Also velocity of advancement of adsorption plane can be calculated as Z/
S
.
CONCLUSIONS:
NOMENCLATURE:
C
0
= Concentration of adsorbate in feed solution, moles solute/mass adsorbent.
I
= Optical density of fluid at exit at time .

V = Velocity of advancement of the adsorption plane, m/s.
X
T
= Adsorbate concentration in equilibrium with entering fluid, moles solute/mass adsorbent.
Z = Actual height of adsorbent column, m.
Z
S
= Length of adsorber bed in equilibrium with feed, m.
17
B
= Time when the color of product start changing rapidly, min.
S
= Time required for idealized breakthrough, min.
T
= Time required for bed saturation, min.
PRECAUTIONS & MAINTENANCE INSTRUCTIONS:
1. Before starting the pump ensure that bypass valve is not fully closed & rotameter is properly
closed.
2. Before starting apparatus check properly that the drain valves of all the columns are properly
closed.
3. It should be ensure that there is no leakage from the bottom of the column.
4. Check properly that only one feed valve is open at a time.
5. The apparatus should be drained off as soon as possible as the color of liquid would clot over the
inner surfaces of the apparatus, making the apparatus yield incorrect results.
6. Pump should not be switched on at low voltage.
7. Carefully note the bed height & initial solution concentration.
TROUBLESHOOTING:
In case of any problem regarding operation of the apparatus; the apparatus should be quickly switched
off and electric supply should be cut off.
Electrical :
Electric shock : It means that either earth wire inside the panel is loose or there is no earth provide in
the socket to which the equipment is plugged. So make it sure that the equipment is earthed properly.
General :
Leakage : The point of leakage should be detected & the concerned part is tightened properly. If the
problem still persists then the part is removed & Teflon tape is wrapped on the threads properly & the
part is then refitted carefully.
==== X ====
18
Experiment No: 03
PERFORMANCE OF
WATER COOLING TOWER
19

PERFORMANCE OF WATER COOLING TOWER
OBJECTIVE:
Study of the heat and mass transfer in Water Cooling Tower for different flow & thermodynamic
conditions.
AIM:
To measure Tower Characteristic parameter( KaV/L) for various liquid and air flow rates(L/G) in a
counter-current Forced draft Cooling Tower. To determine the effect of L/G on [KaV/L] and estimate
the values of mass transfer coefficient Ka for various values of L/G
INTRODUCTION:
Water from condensers and heat exchangers is usually cooled by an air stream in spray ponds or in
Cooling Towers using natural draft or forced flow of air. Mechanical draft towers are of the forced draft
type, where the air is blown into the tower by a fan at the bottom. The forced draft materially reduces the
effectiveness of cooling.
THEORY:
Water may be cooled by the air as long as its temperature is above the wet bulb temperature of the
entering air. Markels theory is used which is based on enthalpy potential difference as the driving force.
Air Output (G, T
3
, T
4
, h
1
) Water In (L, T
5
)
Packing
Cooling Tower
Air In (G, T
1
, T
2
, h
2
) Water Out (L, T
6
)
20
Each particle of water is assumed to be surrounded by a film of air and the enthalpy difference between
the film and the surrounding air provides the driving force for the cooling process. In the integrated form
Markels equation can be written as:
5
6
T
T
h h
dT
L
KaV
Tower characteristic can be evaluated numerically by:
( )
,
_
4 3 2 1
6 5
1 1 1 1
4
5
6
h h h h
T T
h h
dT
L
KaV
T
T a w
h
w1
= value of h
w
at temperature= T
6
+ 0.1(T
5
-T
6
)
h
w2
= value of h
w
at temperature= T
6
+ 0.4(T
5
-T
6
)
h
w3
= value of h
w
at temperature= T
6
- 0.4(T
5
-T
6
)
h
w4
= value of h
w
at temperature= T
6
- 0.1(T
5
-T
6
)
h
a1
=h
1
+ 0.1(L/G) (T
5
-T
6
)
h
a2
=h
1
+ 0.4(L/G) (T
5
-T
6
)
h
a3
=h
2
- 0.4(L/G) (T
5
-T
6
)
h
a4
=h
2
- 0.1(L/G) (T
5
-T
6
)
and
i i
a w i
h h h
The carrying of liquid with gas stream is termed as Liquid Entrainment. This may be due to a high rate
of air flow. This should be avoided to get better performance. This can be avoided by following the
Operational limits of the equipment.
DESCRIPTION:
The apparatus is provided for the process of Forced draft countercurrent cooling of hot water using air.
The water to be cooled is heated in a heating tank using a heater. It is then circulated; through a
rotameter; to the top of the cooling tower mounted over the heating tank. Cooled water is then re-
circulated to the heating tank. A blower is provided for the cooling air. A valve is provided in air line to
regulate the flow rate of air. There is an Orificemeter mounted with its taps connected to a manometer to
find the flow rate of air. A set of two temperature sensors are provided both at inlet and outlet of air
stream. These sensors give Dry bulb and Wet bulb air temperatures. The cooling tower is packed with
Aluminium expanded wire mesh.
Description of the temperature sensors are as follows:
T
1
= inlet dry bulb temperature of air
21
T
2
= inlet wet bulb temperature of air
T
3
= outlet dry bulb temperature of air
T
4
= outlet wet bulb temperature of air
T
5
= inlet water temperature
T
6
= outlet water temperature
UTILITIES REQUIRED:
Water Supply
Drain
Electricity Supply:1 Phase, 220V AC, and 3kW.
Floor area of 1.2m 1m
EXPERIMENTAL PROEDURE:
(1) Fill the heating tank with water, set the temperature with the help of D.T.C and switch on heater.
(2) Switch on pump & blower after desired temperature achieved.
(3) Set the flow rate of water and air.
(4) Record the flow rate of water and manometer reading after steady state achieved.
(5) Record the temperatures.
(6) Steps 3 to 5 may be repeated for different water and air flow rates within operational range.
Operational Parameter Range:
Liquid rate: L=5 to 20LPH
Air rate: G= 10 to 88 mm of manometric difference (with water as manometric fluid)
L/G: 0.75 to 1.5
SPECIFICATION:
Tower : Material Stainless Steel, Size- Cross-section 66, Height 30
Packing : Expanded wire mesh made of Aluminium.
Air Flow Measurement : Orificemeter with U-tube manometer.
Water Flow Measurement : Rotameter
Hot Water Tank : Material Stainless Steel, Double wall, insulated with ceramic wool
Hot Water Circulation : Magnetic Pump made of Polypropylene to circulate Hot Water.
Maximum
working temperature is 85.
Heater : 1.5 kW
Temperature Sensors : 7 No.s
Dry & Wet bulb Temp.-
- Measurement : RTD PT-100 type Sensos
Control Panel comprising of-
Digital Temp. Controller : Range:0-200C. (for hot water tank)
Digital Temperature Indicator: Range:0-200C, with multi-channel switch.
With Standard make On/Off switch, Mains Indicator and fuse etc.
A good quality painted rigid MS Structure is provided to support all the parts.
FORMULAE:
Head in terms of air,
,
_
1
100
air
water
R
H

22
Flow rate of air,
H g C
a a
a a
Q
d

2
2
1
2
2
2 1
0
Mass flow rate of air,
0
Q m
air

Mass flow rate of dry air, G= [m/(1+Y
1
)]/cross-sectional area of column
Rate of humidification= mass flow rate of dry air (Y
2
-Y
1
) kg moisture/sec
DATA:
Orifice dia., d
1
= 34mm
Cross section area of Orifice, a
1
= 9.110
-4
m
2
d
2
= 68mm
Orifice constant, C
o
= 0.6
water
= kg/m
3
air
= kg/m
3
Acceleration due to gravity g = 9.81 m/s
2
Cross section area of Chamber, A = 0.0232m
2
Height of Packing = 0.75m
From the Psychometric Chart for air-water vapor at 1 atm. pressure, determine the following
corresponding to dry bulb and wet bulb temperature of the entering and leaving air:
Y
1
, (corresponding to T
1
and T
2
)
h
1
(corresponding to T
5
)
Y
2
, (corresponding to T
3
and T
4
)
h
2
(corresponding to T
6
)
OBSERVATION TABLE:
S.No R (in m) Flow
rate of
water
(LPH)
Water temp. (C) Air Temperature (C)
Inlet Outlet
h
1
h
2
Inlet Outlet Dry
Bulb
Wet
Bulb
Dry
Bulb
Wet
Bulb
CALCULATIONS:
Calculate flow rate of air Q
0
and mass flow rate of air m
For flow of compressible fluid, mass flow rate is to be multiplied by an Expansion factor .
For the pressure ratio nearly equal to one, = 1
Mass flow rate of dry air, G = [m/(1+Y
1
)]/A kg dry air/h-m
2
Rate of humidification= mass flow rate of dry air (Y
2
-Y
1
)
L/G ratio is calculated from the L & G calculated as above.
The values h
a
are found at different temperatures as below:
T, C h
a,
kJ/kg of dry air
T
6
h
a
=h
1
23
T
6
+0.1 (T
5
-T
6
) h
a
=h
1
+ 0.1(L/G) (T
5
-T
6
)
T
6
+0.4 (T
5
-T
6
) h
a
=h
1
+ 0.4(L/G) (T
5
-T
6
)
T
5
-0.4 (T
5
-T
6
) h
a
=h
2
- 0.4(L/G) (T
5
-T
6
)
T
5
-0.1 (T
5
-T
6
) h
a
=h
2
- 0.1(L/G) (T
5
-T
6
)
T
5
h
a
=h
2
=51.2237
h
w
data is calculated at the specified temperatures from the psychometric chart to calculate h
i
s. Now
according to Markels Theory; the cooling tower characteristic KaV/L is calculated as below:
( )
,
_
4 3 2 1
6 5
1 1 1 1
4
5
6
h h h h
T T
h h
dT
L
KaV
T
T a w
CONCLUSIONS:
NOMENCLATURE:
a = Contact area, m
2
/m
3
of tower volume
A = Cross section Area of Chamber, m
2
a
1
= Cross section area of Orifice, m
2
a
2
= Cross section area of pipe, m
2
C
0
= Orifice constant
d
1
= Diameter of Orifice, m
d
2
= Diameter of pipe in which Orificemeter is installed, m
g = Acceleration due to gravity, m/s
2
G = Mass flow rate of air, kg dry air/s.m
2
G' = Mass flow rate of air, kg air/s.
H = enthalpy of air stream, kJ/kg
h' = enthalpy of saturated air, kJ/kg
h
a
= enthalpy of air-water vapor mixture at its wet bulb temperature, kJ/kg of dry air
h
w
= enthalpy of air-water vapor mixture at bulk water temperature, kJ/kg of dry air
K = mass transfer coefficient, kg of water/h-m
2
KaV/L = tower characteristic parameter
L = flow rate of water, kg of water/h-m
2
M = Mass flow rate of air, kg air/s-m
2

R = Oifice manometer reading (for air flow), m
V = active cooling volume m
3
/m
2
of plan area
V
0
= Velocity of air at Orifice, m/s
Y
1
= Percentage saturation at inlet, kg moisture/kg air
Y
2
= Percentage saturation at outlet, kg moisture/kg air
24
= Coefficient of contraction for Orificemeter
==== X ====
25
Experiment No: 04
WETTED WALL COLUMN
26
WETTED WALL COLUMN
AIM:
To study the rates and phenomena of diffusion into gases flowing through the pipe and also to compare
the results obtained with literature values (Sherwood& Gilliland).
THEORY:
A thin film of liquid falling down the inside of a vertical pipe through which the gas flows, constitutes a
wetted wall column. Wetted wall column have been used successfully as absorbers for Hydrochloric acid
gas, Ammonia, Acetone, Benzene and other volatile liquids. They have also been used for theoretical
studies for mass transfer because the interfacial surface between the phases is kept under control and is
measurable.
The height of a wetted wall column required for many mass transfer operations is excessive and
consequently this is not widely used. Where large quantities of liquid or gas have to be handled it would
be necessary to arrange many vertical pipes in parallel and this leads to difficulties in the distribution of
the liquid into the inner surface of the tubes. The gas pressure drop from this type of equipment is very
low, however since it is almost entirely confined to skin friction effects, with few or no expansion or
contraction losses.
Mass transfer rates for fluids flowing through pipes have been studied more completely than other cases.
The rates of diffusion into gases flowing through pipes have been studied with the help of wetted wall
columns, shown schematically in Figure. A volatile liquid is permitted to flow down the inside surface of
a circular tube, while a gas is blown upward or downward through the center of the pipe.
Measurement of the rate of evaporation of liquid into the gas stream over the known surface permits the
calculation of the mass transfer coefficient for the diffusion of the vapor into the gas stream. Since the
liquids may be pure liquids, the concentration gradient for the diffusion exists entirely within the gas
stream and coefficient K
G
may be obtained directly from the data. Sherwood and Gilliland conducted a
series of experiments of this sort, using a variety of volatile liquids with air in turbulent flow. For
graphical representation refer to Coulson & Richardson volume 2. Here the mass transfer coefficients in
the form of a dimensionless group are plotted against the Reynold number of the gas for the system Air-
Water (S
C
=60).Similar data obtained for volatile liquids is shown in the upper line. For gases, values of
Re from 2000 to 35000 were covered and Sc from 0.6 to 2.5 with gas pressure varying from 0.1 to 3.0
atm.
The average slope of the line in graph is 0.83 so that the groups (K
G
*d/D)* (P
B,M
/P) and (K
L
*d/D) vary as
Re
0.83
. In another graph the intercepts of these lines at Re = 1000 are plotted against the corresponding
values of Sc on logarithmic coordinates. The principal line of this graph has a slope of 0.333. The
equation, which describes all the data, for both the liquid and gas flow, is therefore,
(K
G
*d/D)* (P
B,M
/P)* (K
L
*d/D) = 0.023 Re
0.8
Pr
0.3
This empirical relation is quite remarkable in the manner in which it generally confirms the relationship
between heat, mass and momentum transfer developed theoretically. It should be noted that the
27
evaporation of the volatile liquids in a wetted wall column results in cooling of the liquids
and consequent simultaneous heat transfer between liquid and gas.
The heat transfer rates are somewhat higher than those given by the equation,
H*D/K = 0.023 Re
0.8
Pr
0.3
Owing to ripples and waves on the liquid surface, it should also be noted that data for gases only in
graphs (Sc = 0.6 to 2.5) are correlated empirically better by the relation,
(K
G
*d/D)*(P
B, M
/P) = 0.023 Re
0.83
Sc
0.44
(broken line in the graph)
DESCRIPTION OF EQUIPMENT:
Air is supplied to the column at the bottom by means of blower. Bypass valve V
1
and control valve V
2
are used for varying the airflow rate. The condition of air at inlet and outlet from the column are
measured by the wet bulb and dry bulb thermometer, respectively. Water inlet and outlet temperatures
are measured by the thermometers T
1
and T
2
. A wire mesh screen is placed over the surface of the tube.
Manometer M
1
and M
2
measure the pressure drop across column and air flow rates. Water flow rate is
measured by rotameter readings.
PROCEDURE:
Water is fed to the column at a rate at which complete wetting with a minimum of ripple
formation is visible.
The blower is started and a minimum flow of air is maintained.
After about 5 minutes when steady state conditions could have reached, the humidity of air inlet
and outlet are determined by the readings of the wet and dry bulb thermometers and by the use of
a psychrometric chart.
Water flow rate and inlet and outlet temperatures are recorded.
From steam tables vapor pressure at the water temperature is noted.
OBSERVATION TABLE:
Run No. Air F.R.
(Q
A
) lpm
Water
F.R. (Q
w
)
lpm
AIR TEMPERATURE
Inlet
(C)
Outlet
(C)
t
d1
t
w1
t
d2
t
w2
*** 1 12.7 3 24.9 24 26.7 26.4
***Sample observations
28
CALCULATIONS:
Length of tube L = 1000 mm
Diameter of tube d = 25 mm
Air flow rate = 0.0095 k-mole / sec
Driving force at inlet of air (at bottom)
P
W1
= P
w1
-p
w1
Where,
P
w1
= pure component vapor pressure of water at outlet water temperature T
1
= can be evaluated by using ANTOINE EQUATION.
p
w1
= Partial pressure of water at bottom (can be calculated by using humidity
and pressure relation).
Driving force at outlet of air (at top)
P
w2
= P
w2
-p
w2
Where,
P
w2
= pure component vapor pressure of water at inlet water temperature T
2.

p
w2
= Partial pressure of water at top .
NOTE: The partial pressure can be calculated from the humidity values obtained from psychrometric
chart by using recorded wet and dry bulb temperature of air at top and bottom.
SAMPLE CALCULATIONS:
(for sample observations)

Mean driving force,
P
W,M
= (P
w1
- P
w2
) / ln (P
w1
/P
w2
)

= 0.95 /1.2267
=0.7743
Amount of water absorbed by air (evaporated)
N
w
= Q
A
((p
w2
-p
w1
)/P) K-mole/sec
Where, Q
A
is air molar flow rate (K-mole/s)
= 0.0095*2.5/760
N
W
= 0.00003125
29
Wetted surface in the column = A = *d*L (m
2
)
Where,
d = ID of the column
L = Effective length of the column
In terms of mass transfer coefficient Kg the rate of mass transfer is given by,
N
w
/A = K
G
*(P
B, M
)
K
G
= N
W
/ (A*P
B,M
) k-mole/m
2
.s.mm Hg
= 0.00003125/3.14*0.0254*0.7743)
= 0.0005060 k-mole/m
2
.s.mmHg
CONCLUSIONS:
NOTES:
(1). ANTOINE EQUATION:
lnP = A-B/(T+C)
where,
A = 18.3036; B = 3816.44; C = -46.13 (for water)
(2). PERRYS EQUATION (HUMDITY RELATION FOR PARTIAL PRESSURE)
H = [p
w
/(P-p
w
)]*(M
water
/M
air
)
Where,
H = absolute humidity
P = atm. pressure
M
water
= 18 kg/Kg-mole
M
air
= 29 Kg/Kg-mole
==== X ====
30
Experiment No: 05
DIFFUSION COEFFICIENT OF
ACETONE (VAPOR) IN AIR
31
DIFFUSION COEFFICIENT OF ACETONE (VAPOR) IN AIR
AIM:
To determine diffusion coefficient or diffusivity, of given liquid (acetone) in air by using ARNOLDs
cell.
APPARATUS:
Arnolds cell, Thermometer and Scale for measuring drop in height of solvent.
CHEMICALS: Acetone
THEORY:
This is the case of pseudo-steady state diffusion in which one of the boundaries shift with time the effect
that the length of the diffusion path changes, though only by a small amount over a long period of
exposure.
When this condition exists:
The molar flux at any instant in the gas phase

N
A,Z
= (D
AB
/Z)(P/RT)(1/P
B,lm
)(P
A1
-P
A2
)
Where,
Z = Z
1
- Z
2
= the length of the diffusion path in time t.
The molar flux of A leaving the liquid at any instant
N
A,Z
= (
A,L
/M)(dz/dt)
(
A,L
/M)(dz/dt) = (D
AB
/Z)(P/RT)(1/P
B,lm
)(P
A1
-P
A2
)
Where
A,L
/M = molar density of air liquid phase
Under pseudo-steady-state conditions,
D
AB
(P/RT)(1/P
B,lm
)dt = (
A,L
/M)Zdz
Upon integration this yields
(D
AB
)(P/RT)(1/P
B,lm
)(P
A1
-P
A2
)t=(
A,L
/M)(1/2)(z
1
2
-z
2
2
)
PROCEDURE:
Acetone is filled in capillary tube and air bubble, if present, is removed from the tube carefully.
Note down the initial height (H
0
) of the acetone level in the tube.
32
The tube is placed in a water bath to maintain the constant temperature. Note down the
temperature of the water by thermometer.
Switch on blower, which blown air across the opening of capillary tube continuously to remove the
vapors evaporated that rises from the surface of the liquid.
At regular interval of time note down the drop in the level of acetone.
Do necessary calculations and find out the diffusivity (D) from the equation.
Also calculate the diffusivity from the GILLILANDs equation (as given below) at the same
temperature using standard data and compare the result with the experimental one.
Repeat the same procedure for two-three different temperatures by increasing and maintaining
constant temperature of the water bath and calculate the diffusivity by both the methods. State your
conclusion precisely at the end.
D = (4.310
-4
)(T)
1.5
(1/M
A
+1/M
B
)
0.5
/(P(V
A
1/3
+V
B
1/3
))
OBSERVATION TABLE:
SR.NO. TEMP (C) INITIAL HEIGHT
OF LIQUID (mm)
FINAL HEIGHT OF
LIQUID (mm)
TIME (Sec.)
CALCULATIONS:
1. Vapor pressure of acetone at given temp.
P
A1
= ___________________ mm Hg
2. P
B1
= P-P
A1
3. P
A2
= 0 (Since pure B(air) is flowing)
4. P
B2
= P-P
A2
P
B,lm
= (P
B2
-P
B1
)/ln(P
B2
/P
B1
)
5.
A
= ______________________kgmol/m
2
sec
6. Z
1
= __________cm , Z
2
= __________cm
7. D
AB
= ___________ m
2
/sec
DATA:
1. P = 1 Std. atm = 760 mm Hg = 101325 N/m
2
2. R = 8314 N. m/kmol K
3. Room Temp = ________C
33
4. Density of acetone
5. Molecular wt. of acetone___________kg/m
3
DIFFUSIVITY BY GILLILANDs METHOD:
D = (4.310
-4
)(T)
1.5
(1/M
A
+1/M
B
)
0.5
/(P(V
A
1/3
+V
B
1/3
))
V
A
= molar volume of acetone
= ________________m
3
/kmol
V
B
= molar volume of air
=_________________m
3
/kmol
M
A
= molecular weight of acetone
=_________________kg/kgmol
M
B
= molecular weight of air
= _________________kg/kgmol
T = Absolute temp.
=__________K
D = ____________m
2
/sec from Gillilands equation
RESULTS:
CONCLUSIONS:
==== X ====
34
Experiment No : 06
GAS ABSORPTION IN
MECHANICAL AGITATOR
35
GAS ABSORPTION IN MECHANICAL AGITATOR
AIM:
To find the absorption efficiency of the mechanical agitator vessel.
THEORY:
The process of absorption of the gas in the liquid is really entirely a physical one. However in number of
cases in which the gas on absorption reacts chemically with a components of the liquid phase. Thus in
absorption of CO
2
by NaOH the CO
2
reacts directly with the NaOH and the process of absorbed in
Ethanolamine solutions there is direct chemical reaction between the Amine and the gas. In such cases
there is a liquid film followed by a reaction zone.
The effective interfacial area a in the gas liquid contractor is an important mass transfer characteristic in
the design of the contractor.
The system used in this experiment is a gaseous solvent A dissolving in a liquid acid simultaneously
reacting with the reactant B present in the liquid phase.
A + bB AB Products
The new products AB formed diffuse towards the main body of the liquid. The concentration of B at the
interface falls; this results in diffusion of B from the bulk of the liquid phase to the interface. Since the
chemical reaction is rapid, B is removed very quickly so that it is necessary for the gas A to diffuse
through the part of the liquid film before meeting B. There is thus a zone of reaction between A and B
which moved away from the gas liquid interface taking up some position towards the bulk of the liquid.
The final position of the reaction zone will be such that the rate of diffusion of A from the gas liquid
interface is equal to the rate of diffusion of B from the main body of the liquid. When this condition has
been reached the concentration of A, B and AB can be indicated as shown in the figure.
According to the film model if the reaction is fast enough the solute A will be consumed by the reaction
in the liquid film itself and its concentration will be zero at the end of the liquid film. The condition for a
fast second order reaction is,
[ ] ( )
O A A
B K D * *
2
/
L
K >3 (1)
Where,
D
A
- Diffusivity of A, m
2
/ sec
K
A
- Second order reaction constant, m
3
/kmol. Sec
[B
o
] - Concentration of B in bulk liquid, kmol / m
3

K
L
- Liquid side mass transfer coefficient, m /sec
36
In such a case the reaction occurs simultaneously with the diffusion process in the liquid film and
therefore enhances the rate of absorption significantly. If the reactant B is present in far excess of the
stoichiometric requirements for the reaction in the film, then the depletion of the reactant concentration
in the film is negligible. The condition for such a case is given by,
[ ] ( ) [ ] ( ) [ ] ( ) * * / * / * *
2
o A o B L o A A
A b D B D K B K D << (2)

Where
[ ] *
o
A
is equilibrium concentration of a.
Under such conditions the reaction can be considered to be pseudo first order with respect to the solute
A, and the volumetric rate of absorption of A is given by,

[ ] [ ]
o A o A
B K D A a a R * * * *
2
*
(3)
From the equation (1) it is clear that the rate of absorption is a unique function of the physico-chemical
properties and completely independent of the hydrodynamics of the system.
The absorption of carbon dioxide by caustic soda or potash is accompanied by an irreversible chemical
reaction and the partial pressure of CO
2
in equilibrium with the solution is zero. The reaction with
sodium carbonate to form sodium bicarbonate is reversible; the equilibrium partial pressure depends on
the normality of the solution (as Na
2
CO
3
+ NaHCO
3
), on the fraction of carbonate converted to
bicarbonate and on the temperature. This relation may be expressed graphically (Sherwood and pigfor,
1952) or by the equation,
( ) ( )( ) t f N f p 365 1 / 137
29 . 1 2
Where,
P is the equilibrium partial pressure, mm. of mercury,
N is the normality,
f the fractional conversion to bicarbonate,
t the temperature,
0
F
and S is the solubility of pure CO
2
in water at a pressure of 1 atm, in gmole/litre.
The equation may be used also to determine the partial pressure in equilibrium with potassium carbonate
bicarbonate solutions. If the constant 137 and 365 are replaced by 45 and 302 respectively.
The absorption of carbon dioxide is followed by a hydrolysis reaction in solution which can be
represented by the equations:

+
3 2
HCO OH CO I
+
+ +
3 2 2
HCO H O H CO II
37
The reaction rate constants determined by Himmelblau and Babb (1958) at 20
0
C are
Reaction I k = 2.77
105 sec
-1
Reaction II k = 0.0149 sec
-1
The first reaction is operative in the absorption of carbon dioxide by caustic solutions. Since this is a fast
reaction the factors controlling the absorption are the rates of diffusion of the reactants in the liquid
phase. The second reaction is slow and controls the rate of absorption in carbonate solutions. Nijsing et
al. (1958, 1959) have investigated the kinetics of absorptions by caustic and carbonated solutions in
Wetted-wall columns and Danckwerts and Kenddedy (1959) discuss the results obtained from
experiments of absorption in a liquid film on a rotating drum. The experimental results on the absorption
of carbon dioxide by alkaline solutions are usually expressed as the overall gas film coefficient because
the concentration gradient in the liquid is unknown. Justification of this procedure is afforded by the
work of Pozin (1947) who showed that the rate of absorption in a batch absorber was proportional to the
partial pressure of carbon dioxide in the gas phase.
The results of spector and Dodge show that the coefficient K
G
a is inversely proportional to the square
root of the absolute gas pressure and tends to decrease as the packed height is increased. The data
showed good agreement with results from a commercial installation. The coefficients for caustic potash
solution were 20 to 30 % higher than those for caustic soda of the same normality.
The dependence of the coefficient on the gas flow rate is an indication that at very low concentrations
the absorption of carbon dioxide is partially controlled by the gas phase coefficient. Tepe and dodge
(1943) showed that at higher concentrations (2% CO
2
) the absorption is wholly controlled by the liquid
film. The coefficient was independent of the gas rate and proportional to the 0.28 power of the liquid
rate.
Effect of temperature and the effect of the sodium hydroxide concentration and the degree of conversion
to sodium carbonate. The coefficient value when the total sodium concentration is 1.8 normal.
The effect of varying the carbon dioxide concentration in the gas phase over a rang e form 3 to 28% has
been investigated by Blum, Stutzmanb and Dodds (1952). The overall gas film coefficient, K
G
a was
found to be independent of the gas flow rate but dependent on the liquid flow rate, the concentration
(normality) of the alkali, and on the partial pressure of carbon dioxide in the gas. The experiments of
absorption in sodium hydroxide solution showed that K
G
a increased with the normality of the sodium
hydroxide up to 1.5N, but was not affected by a further increase in concentration.
The effect of the partial pressure of the carbon dioxide was a function of the normality of the liquid. At
high normality (above 1.5 N) K
G
a decreased as the average partial pressure had no effect on the
coefficient. At lower normality (0.99 N) the coefficient decreased as the partial pressure increased
throughout the range of the experimental data. The coefficient decreased progressively as the sodium
hydroxide was converted to carbonate. The volumetric coefficient, K
G
a appeared to be independent of
the packing size. The coefficients of absorption of carbon dioxide in potassium hydroxide were
appreciably higher than those for sodium hydroxide under equivalent conditions. It was assumed that the
following chemical reactions occur in solution:

+
3 2
HCO CO OH

+ +
3 2 3
CO O H HCO OH

+ +
3 2 2 3
2HCO O H CO CO
38
The second reaction was throught to be rapid and the third reaction irreversible in the presence of OH
-
ions. The rate of absorption Na (lb.mole/hr.) in a tower of unit cross section (1ft
2
) and height h (ft.)
( )( ) ( )
m
CO OH h K Na ' / '
3

Where K is a function of the liquid rate and is the lonic strength of the solution. A satisfactory
correlation of the results was obtained when
m = 1.09
K = 0.0176L
0.84
Where L is the liquid flow rate in lb.Mole/(hr.)(ft2)
The absorption of carbon dioxide by sodium and potassium carbonate solutions has been studied by
Payne and Dodge (1932), Comstock and Dodge (1937) and Furnas and Bellinger (1941). The rate of
absorption is controlled by a slow chemical reaction in the liquid phase. It is independent of the gas rate
and decreases with increasing normality of the solution and with conversion of the carbonate to
bicarbonate. Payne and Dodge noted that the coefficient is approximately proportional to the liquid hold-
up in the tower.
One of the most important industrial applications of carbon dioxide absorption lies in the production of
synthesis gas for synthetic ammonia or the manufacture of hydrocarbon products by the Fischer-Tropsch
process. The synthesis gas, which may be produced by the partial combustion of natural gas or by the
gasification of coke in producer gas or water gas plants, contains a high proportion of carbon dioxide
which must be removed by absorption in a suitable solvent. To overcome the relatively low solubility of
carbon dioxide, the absorption is usually carried out at a pressure of 10 to 50 atm. At high pressure it is
possible to remove the carbon dioxide by solution in water, but this has the disadvantage that the
pumping costs are high owing to the large quantities of water which must be circulated through the
absorption towers. The liquid flow rates can be reduced by absorbing the carbon dioxide in a solution of
sodium or potassium carbonate or mono-or diethanolamine. The solution is regenerated by heating at a
lower pressure to drive off the carbon dioxide.
Benson, Field and Jimeson (1954) Benson, Field and Haynes (1956) have discussed the relative merits
of carbonate and amine solutions for the removal of carbon dioxide from synthesis gas at 300 lb / in
2
pressure. Potassium carbonate is preferred to sodium carbonate owing to its greater solubility in water
and the reduced risk of deposition of solid bicarbonate in the absorber. A comparison of potassium
carbonate and mono-ethanolamine showed that the farmer had two important advantages; less heat is
liberated in the absorber owing to the smaller heat of solution of carbon dioxide in potassium carbonate
solution, and the regeneration can be carried out at a lower temperature. This made it possible to carry
out the absorption and regeneration of potassium carbonate solution over the same temperature range
(225 to 240
0
F) and considerable savings in heat could be effected. The absorption was carried out at a
gas pressure of 300 lb / in
2
and the solution regenerated by reducing the pressure to 5 lb / in
2
gauge and
stripping the solution with steam.
39
PROCEDURE:
Initially start the air compressor and collect sufficient air in the pressure tank so as the pressure is
about 3-4 kg/cm
2
. Prepare the dilute NaOH solution in the tank. Open the valve of the pressure
tank and allow the air to pass through the column. Set the air flow at the desired value and then
open the valve on the CO
2
cylinder and adjust the flow rate to predetermined value. After
sometime take the sample at various points (liquid as well as gas) and analyze them.
Initially start the liquid flow at sufficiently high rate to ensure that the agitation in the vessel
should be well.
The flow rates of gas and liquid are adjusted at predetermined values. The CO
2
flow rate should
be such that the % CO
2
in the mixed gas is about 8-10%. The gas velocity has no effect on the
interfacial area in a vessel.
Hence a value of V
G
between 0.1-0.2 m/s may be chosen for all the experiments and keeping it
constant. The linear superficial liquid velocity V is the most important variable. The range for V
should be fixed between 0.001-0.007 m/s.
The system is allowed to reach steady state after fixing the liquid level in the bottom section at a
marked height. Inlet and outlet liquid samples are withdrawn for analysis. This procedure is to be
repeated for 6-7 different values of V
L
chosen in such a way that the range indicated is fully
covered.
OBSERVATIONS:
System (CO
2
+ Air) - Aq. NaOH Solution
Agitator used - Flat blade turbine
Vessel Dia - 300 mm
Vessel Height - 400 mm
Turbine Dia - 100 mm
Turbine width - 20 mm
Sparger type - Ring
Number of holl - 8
Holl Dia - 3 mm
Ring Dia - 90 mm
Chemical Reaction:
CO
2
+ NaOH NaHCO
3
NaHCO
3
+ NaOH Na
2
CO
3
+ H
2
O
Final Reaction:
2NaOH + CO
2
Na
2
CO
3
+ H
2
O
Here, NaOH is excess material so stochemetrically reaction is 2:1 ratio.
OBSERVATION TABLE:
40
Sr. No. Flow rate of
Air LPM
Flow rate of
CO
2
LPM
Burette
Reading ml
Time Sec.
41
CALCULATION:
The concentration of NaOH used should be between 2 2.5 g mol/lt. The inlet CO
2
percentage is
kept around 10%. Under these conditions the equations (1) and 92) are satisfied and the
absorption of CO
2
is accompanied by a fast pseudo first order reaction.
5 ml of sample (or 10 ml) is titrated against standard HCl of molarity (approx. 1 gmol/litre) using
phenolphthalein as an indicator. Titrate Value (V
1
) = . ml.
Initially feed of NaOH in gmol/min.
Feed normality of NaOH solution is = gmol/min.
After steady state titrate the product with 0.1 N HCl solution use phenolphthalein as an indicator.
gmmoles of CO
2
in feed = [(Flow rate*10
-3
*density) / Molecular weight] * 1000
= [(...*10
-3
*1.5) / 44] * 1000
= . mmmoles / min.
gmmoles of NaOH in feed
= Normality of feed
=
=
Burette reading = . ml
So, NaOH consumed = . gm moles / min
CO
2
absorbed = . gm moles / min
(because stochiometrically this is 2:1 ratio)
% CO
2
absorbed = (CO
2
reacted / CO
2
feed) * 100
= ( .. / ..) * 100
=
RESULT:
CONCLUSION:
==== X ====
42
Experiment No : 07
BATCH CRYSTALLIZATION
43
BATCH CRYSTALLIZATION
OBJECTIVE:
Study of crystallization
AIM:
To study the crystallization of MgSO
4
.7H
2
O in a batch crystallizer.
To verify the material balance around the crystallizer.
To determine the yield of MgSO
4
.7H
2
O crystals.
INTRODUCTION:
Crystallization is the formation of solid particles within a homogeneous phase. Its wide use has a two-
fold basis, a crystal formed from an impure solution is itself pure and crystallization affords a practical
method of obtaining pure chemical substances in a satisfactory condition for packing and storing. This
operation involves both heat and mass transfer.
THEORY:
Crystallization is the process whereby a solid separates from a solution because conditions have been
imposed on the solution to allow the solid phase to form and particles of crystalline character to grow to
a size sufficiently large to allow separation by physical methods.
A saturated solution containing the solute is altered by either cooling, evaporation of solvent, or addition
of another substance so that the ability of the solvent to dissolve the solute is lessened, and a fraction of
the solute forms a solid phase, which may be removed from the mixture.
From the solubility or phase diagram the effect of changes in the temperature and solute and solvent
concentrations can be seen.
Based on the material balance, the yield of crystals resulting from cooling and or loss of solvent due to
evaporation can be estimated from:
( ) [ ]
( ) 1 1
1
2
2 1

R C
V C C WR
Y
The physical properties of saturated solutions and slurries may be obtained from:
( )
p F
F p
s
X X

1
Viscosity:
44
( )
( )
64 . 0
1
1 . 4
e
f s
( In many cases slurries have20% solids, 8 . 0
8 . 1
f
c
SATURATED SOLUTION:
A saturated solution is a solution which is in equilibrium with a solid phase of the dissolved material. A
saturated solution has in it the maximum quantity of the solute at that temperature.
If the saturated solution is cooled or solvent evaporated, a non-equilibrium condition is established
which can be remarkably stable. That is, a solid phase will not immediately precipitate in order to re-
establish the equilibrium. This non-equilibrium solution where in the liquid has dissolved more than the
equilibrium quantity of solute is called super saturated solution.
The super saturation of a given solution cannot become infinitely large. There is a limit. This limit is
encountered when there occurs a spontaneous formation of solid crystals known as nuclei.
If these nuclei are allowed to grow, crystals are formed and the system reverts to the equilibrium state.
The process of crystallization is show in figure:
1. A saturated solution can be made
supersaturated by a change of temperature
(cooling) or a reduction in solvent content.
This supersaturated solution can remain in
a meta-stable equilibrium for very long
period of time.
2. In the meta-stable zone crystal growth can
occur if there are seed crystals upon which
the solids may deposit, but spontaneous
nucleation will take place.
3. In the labile zone there will be a sudden
spontaneous formation of crystal nuclei that
will produce so many very small particles.
Unstable region of
Nucleatic
Metastable & -
Supersaturated
2
1
Stable &
Unsaturated
Temp.
Coolin
g
Equilibrium Solubility
BATCH CRYSTALLIZATION: Batch crystallization is characterized by the fact that the system is
always in the unsteady state. The initial super saturation at which crystallization starts will drop quickly
45
from relatively high value to the saturation value. If crystal growth is to continue, the
solution must be maintained in the meta-stable region. As a consequence, cooling must continue and the
batch temperature must continue to drop during the growth period. In batch crystallization it is
comparatively easy to penetrate the labile zone producing a fine mass of fine crystals. By using
controlled seeding the solution will not become labile thereby aiding crystal growth.

T vs Concentration
50
45
40
35
30
25
20
15 C = 0.494 T + 25.85
10
05
0

0 5 10 15 20 25 30 35 40 45
T (
0
C)
DESCRIPTION:
Cooling type agitated batch crystallizer set up consists of an open jacketed stirred vessel provided with
water heating and cooling arrangement. The feed is prepared in the crystallizer itself with hot water and
stirrer. The hot super saturation solution in the crystallizer is then cooled by circulation of cooled water
and crystals are formed.
UTILITIES REQUIRED:
Water Supply
Drain
Electricity Supply: 1 Phase, 220V A.C, 1.5kW
Required Chemicals: MgSO
4
.7H
2
O
1. Prepare a saturated solution of MgSO
4
.7H
2
O in water at 80C by dissolving 66.2gm
MgSO
4
.7H
2
O in 100gms of solution (1.9856gm MgSO
4
.7H
2
O per gm of free water). The crystallizer
should be filled to 3/4
th
the capacity. Prepare about 1.5L of solution of MgSO
4
.7H
2
O and water.
During mixing, the agitator should be used for effective mixing.
2. After uniform mixing has been achieved, stop the electric supply to the electric heater.
3. Allow the flow of cold water (20C) to pass through the jacket at a pre-fixed flow rate with the
help of water by-pass valve & a Rotameter. Record the flow rate (flow rate may be fixed such that
the rise in cooling water temperature is maximum around 5-7C maintain by using ice.)
46
C
o
n
c
e
n
t
r
a
t
i
o
n

(
g
m

s
o
l
i
d

/

g
m

s
o
l
u
t
i
o
n
)
4. Record the temperature of inlet water and solution temperature with the help of
respective sensors.
5. Put 10gm MgSO
4
.7H
2
O in the crystallizer when the temperature rises to 50C for seeding.
6. Carry out the crystallization process for about 2 hours.
7. After 2 hours, stop the cooling water supply, open the valve fixed at the cone of the crystallizer
and collect the slurry in the bottom receiving tank that is fixed with a mesh at the top. The crystals
shall be collected on the mesh and liquid in the tank.
8. Collect all the crystals from the mesh on a filter paper and weigh. Let the weight of the product
crystals be P (kg). For collecting all the crystals you may flush the crystallizer tank with 100-200ml
of saturated MgSO
4
solution.
9. Steps 1-8 may be repeated with the addition of known weight of seed crystals at step 6.
10. Steps 1-8 may also be repeated for different values of cooling water flow rates.
SPECIFICATION:
Crystallizer = Material SS, Capacity: 2Ltrs with (jacketed) conical bottom.
Stirrer = FHP
Heater = Nichrome Wire Heater
Cooling Water Tank = Material SS, Capacity 30 Ltrs, fitted with
pump
Flow measurement = Rotameter for cooling water
Pump = FHP
Receiving Tank = Material SS, Capacity 2Ltrs, with SS sieve
Piping = SS and PVC
Temp. Sensors = RTD PT-100 type
Control Panel consists of:
Digital Temp. Indicator = 0-199.9C, RTD PT-100 Type with multi-channel switch
With Standard make on/off switch, Mains Indicator etc. the whole set up is well designed and arranged
in a good quality painted structure.
FORMULAE:
Amount of wet crystals of MgSO
4
.7H
2
O collected after 2 hrs = P kg
Crystal yield = Feed Mother Liquor

This must be equal to P the observed yield.
% Recovery = P/ (Crystal Yield)
ld CrystalYie
P
ery cov Re %
OBSERVATIONS AND CALCULATIONS:
Sample Observations and Calculations:
DATA:
Concentration of feed solution of MgSO
4
.7H
2
O at 80C = 66.2gm/100gm of solution
Wt. of Feed solution, F = 2.9856gm
MgSO
4
.7H
2
O = 1.9856gm
Free Water = 1.0000kg
Solubility of MgSO
4
.7H
2
O at 20C = 53.8gm/100gm of solution
47
= 1.1645 gm
MgSO
4
.7H
2
O/gm of water
Wt. of MgSO
4
.7H
2
O taken = 2.9856 kg
Amount of water added = 1.9856 kg
Conc. of feed solution at 50C = 1.9856 gm MgSO

4
.7H
2
O per gm of
free water
= 0.662 gm MgSO
4
.7H
2
O in 1 gm of
solution
OBSERVATIONS:
Time T, min Cooling Water Solution Temperature, T
s
C
Inlet, T
wi
Outlet, T
wo
Amount of crystal MgSO
4
.7H
2
O collected after 2 hours = P kg
Wt. of mother liquor = M kg
CALCULATIONS:
Initial conc. of feed, C1 = 0.662 MgSO
4
.7H
2
O per gm of solution
At 80C solubility of MgSO
4
.7H
2
O = 0.662 gm/gm of solution
Applying material balance:
Final amount of soluble MgSO
4
.7H
2
O in the solution
gmOfWater
O H gmMgSo
) 662 . 0 1 (
7 . 662 . 0
2 4
= 1.9586 gm MgSO
4
.7H
2
O /gm of water
MATERIAL BALANCE:
Total MgSO
4
.7H
2
O Free Water MgSO
4
.7H
2
O
Free Water
Feed
Mother liquor

Material balance as expressed in the table can be compared with the actual quantities recorded during the
experiment. Discrepancy if any should be accounted for.
Amount of wet crystal of MgSO
4
.7H
2
O collected after 2 hours, P = ---------kg
Crystal Yield = ---------kg

This must be equal to P the observed yield.
48
% Recovery = 100
305 . 3

P
CONCLUSIONS:
NOMENCLATURE:
C
1
= Initial solution concentration, kg of anhydrous salt/kg of solvent.
C
2
= Final solution concentration, kg of anhydrous salt/kg of solvent.
R = Ratio of molecular wt. of hydrate and anhydrous salt.
V = Solvent lost by evaporation kg/kg of original solvent.
W = Initial wt. of solvent (Water), kg
X = Wt. fraction of solids in slurry.
Y = yield of crystal, kg
c
= density of crystal, kg/m
3
f
= Fluid density, kg/m
3
p
= solid particle density, kg/m
3
s
= slurry density, kg/m
3
s
= Viscosity of slurry, cP
f
= Viscosity of saturated solution, cP
= Fraction of liquid in slurry.
PRECAUTIONS AND MAINTANENCE INSTRUCTIONS:
1. For proper crystallization feed solution should be saturated.
2. During cooling the temperature should be near to 0C.
3. Priming or seeding should be done at 40-45C.
4. Dont switch on the heater before filling the feed solution in the crystallizer.
5. Proper cleaning is necessary with hot water.
TROUBLESHOOTING:
1. If any type of suspended particles comes in the rotameter, then remove the rotameter, clean the
tube and then fit it at its place.
2. If there is any leakage, tight that part or remove that and re-fix that again after wrapping Teflon
tape.
3. If D.T.I display I on display board it means sensors connection are not O.K tight that.
4. If switch ON the heater but temperature cant rise but panel LED is ON it means bath heater had
burned replace that.
==== X ====
49
Experiment No: 08
DIFFERENTIAL DISTILLATION
50
DIFFERENTIAL DISTILLATION
AIM:
To verify Rayleighs Equation by carrying out differential distillation of Binary Mixture.
THEORY:
Differential distillation is a batch operation. The operation is used to separate a liquid mixture whose
components have fairly large difference in their boiling points. This type of distillation is frequently
employed in laboratory to concentrate one component in the distillate or residue and where some loss of
the material is tolerated.
Differential distillation is a process of infinite number of successive steps, where, in each step an
infinitesimal portion of a liquid is vaporized and the resulting vapor, which is in equilibrium with the
liquid, is removed. Distillation is continued until the desired composition of the distillate is obtained.
Rayleigh developed a mathematical equation to give the composition of the distillate and the bottoms.
BINARY DIFFERENTIAL DISTILLATION:
Let L be the number of moles of the mixture at a given instant. Let x be the mole fraction of more
volatile components in liquid mixture.

Let y* be the mole fraction of more volatile component in vapor. Y* is in equilibrium with x.
If dL differential amount of liquid vaporized, then by applying the material balance with respect to the
more volatile component we get:
Lx =(L-dL)(x-dx)+y*dL
=L x-x dL -L dx + dL dx + y*dL
Omitting the product dx.dL, we get:
Y*dL = xdL + Ldx
dL(y*-x)= Ldx

(dL/L) = ( dx/y*-x)
The boundary conditions are:
Initially, L = F and x = x
F
; F = moles of feed mixture
Finally L = B and x = x
B
; B = moles of bottom mixture
(dL/L)= (dx/y*-x)

ln(F/B)= (dx/y*-x)
51
Using the vapor-liquid equlibrium data for the binary system, the plot is made of 1/(y*-x) vs. x. Area
under the curve between the ordinates at x
B
and x
F
gives the value of the integral on the R.H.S. of the
above equation.
From this we can obtain the value of B, the amount of bottoms to be left to attain the given composition
x
B
of the liquid. Alternatively if we want to calculate the composition of bottoms, when B is known, then
L.H.S. of the above equation can be found out and value of x
B
adjusted to obtain the area under the curve
equal to ln (F/B).
For an ideal system, relative volatility is constant. Therefore for an ideal system we can use:
y* = ( x /1 + ( -1)x)
Substituting the value of y* in equation
ln(F/B) = (dx/(( x/1+( -1)x)-x)
= (1/( -1)(1/x +/(1-x)dx

ln(Fx
F
/Bx
B
) = ln(F(1-x
F
)/B(1-x
B
))
Both these equations are known as Rayleighs equations.
EXPERIMENTAL SETUP:
The experimental set up to study the differential distillation consist of a 2000 ml single neck round
bottom flask with suitable heating mantle (with sun wig regulator to control the temperature, ON/OFF
switch and indicator lamp), a still head with thermo-pocket (to measure the temperature) is provided
over the flask to route the vapors emerging from the flask to the Lei big type water condenser 400 mm
long). Condensed vapors are collected in collecting beaker and the entire assembly is supported with the
help of a stand.
1. The distillation assembly is charged with 700-750 gm of binary mixture after noting the
refractive index with the help of Abbes Refractometer.
2. The heating mantle is turned ON with the regulator set near to 40% and the condenser water is
then started.
3. The distillation is continued for sufficient time so that 70% of the distillate is collected.
4. The weight of the bottoms and refractive index is noted after cooling down to room
temperature. Similarly the weight and refractive index of the distillate is noted.
5. Using Abbes Refractometer prepare a graph of the more volatile component vs. refractive
index. For this initially take 10 ml of comp. A and 90 ml of component B. Measure the
refractive index and convert the composition of the mixture in mole fraction. Repeat the same
for (20+80, 30+70, 40+60, 50+50, 60+40, 70+30, 80+20, 90+10). You will find this plot to be a
52
linear one and this can now be used to determine the composition in terms of mole
fraction once the refractive index is known.
OBSERVATION AND CALCULATIONS:
Weight of sample feed = W
F
= kg; F = kg mole
Weight of bottoms = W
B
= kg; B = kg mole
Weight of distillate = W
D
= Kg; D = kg mole
Composition of feed = X
F
= mole fraction
Composition of Bottoms = X
B
= mole fraction
Composition of Distillate = X
D
= mole fraction
Plot 1/(y-x) vs. x and calculate x
B
.
Compare the value of x
B
obtained graphically with the experimental value.
Use the equation with relative volatility () assuming it to be as constant and calculate the x
B
and
compare it with experimentally obtained value.
To find mol. Fraction of water (molar volatile component) in feed
1) Normality of Acetic Acid (A.A.) solution.

N
1
V
1
= N
2
V
2
2) Weight of A.A. in feed solution

= 31.05
3) Weight of water in feed solution

= Total wt. of feed- wt. of A.A.
= 230-31.05 = 198.95 gms.
Total moles of feed solution F
= (31.05/60.05)+ (200/ 18) = 11.628
4) Mol. Fraction of water in feed solution (x
F
)
53
= (200/18)/11.628 = 0.955
To find mole fraction of water (molar volatile component) in distillate in residue after distillation.
1) Normality of residue
N
1
V
1
= N
2
V
2
N
1
= 115.2/5 = 3.04 N
Wt. of A.A. in feed solution
= Normality Eq. weight vol. of solution
= 3.04 60.050.058
= 10.58 gms.
2) Wt. of water in residue solution
= Total wt. of residue- wt. of A.A.
= 58- 10.58
= 47.41 gms.
3) Total moles in residue
= (10.58/60.05) + (47.41/18)
= 2.8099
4) Mole fraction of water in residue (x
W
)
= (47.41/18)/2.8099
= 0.9373
For Rayleighs Equation
Ln(F/W) = ln(2.633/2.8099)
= 0.9329
CONCLUSIONS:
54
==== X ====
55
Experiment No: 09
ABSORPTION IN
PACKED BED COLUMN
56
ABSORPTION IN PACKED BED COLUMN
AIM: To determine the absorption efficiency of the packed bed column.
THEORY:
The process of absorption of the gas in the liquid is entirely a physical one. However in number of cases
in which the gas on absorption reacts chemically with a component of the liquid phase. Thus in
absorption of CO
2
by NaOH the CO
2
reacts directly with the NaOH and the process of mass transfer is
made much more complicated. Similarly when CO
2
is absorbed in Ethanolamine solutions there is direct
chemical reaction between the Amine and the gas. In such cases there is a liquid film followed by a
reaction zone.
The effective interfacial area a in the gas liquid contactor is an important mass transfer characteristic in
the design of contactor. In the case of packed column a is determined by the velocity of the liquid
(dispersed phase) and properties like wetting characteristic of packing etc. this experiment is designed to
verify the theory of absorption accompanied by a fast chemical reaction. Due to fast chemical reaction
the concentration of CO
2
is bulk of the liquid is always zero and hence the liquid phase residence time
need not be determined.
In packed column a increases very rapidly with V
L
initially (at low values of V
L
in the range of 0.001-
0.004 m/s). The increase in a become less significantly at higher values of V
L
and eventually the lot of a
Vs. V
L
flattens. The value of V
L
beyond which there is no significant increase a is called the minimum
wetting velocity (MWV).

The system used in this experiment is a gaseous solvent A dissolving in a liquid acid simultaneously
reacting with the reactant B present in the liquid phase.
A + bB AB Product
The new product AB formed diffuses towards the main body of the liquid. The concentration of B at the
interface falls, this results in diffusion of B from the bulk of the liquid phase to the interface. Since the
chemical reaction is rapid, B is removed very quickly so that it is necessary for the gas A to diffuse
through the part of the liquid film before meeting B. there is thus a zone of reaction between A and B
which moved away from the gas liquid interface taking up some position towards the bulk of the liquid.
The final position of the reaction zone will be such that the rate of diffusion of A from the gas liquid.
Interface is equal to the rate of diffusion of B from the main body of the liquid. When this condition has
been reached the concentration of A, B and AB can be indicated as shown in the figure.
According to the film model if the reaction is fast enough the solute A will be consumed by the reaction
in the liquid film itself and its concentration will be zero at the end of the liquid film. The condition for a
fast second order reaction is,
[ ] ( ) 3 / * *
2
>
L O A A
K B K D -- (1)
Where,
57
D
A
Diffusivity of A, m
2
/sec
K
A
Second order reaction constant, m
3
/kmol.sec
[B
O
] Concentration of B in bulk liquid, kmol/m
3

K
L
Liquid side mass transfer coefficient, m/sec
In such a case the reaction occurs simultaneously with the diffusion process in the liquid film and
therefore enhances the rate of absorption significantly. If the reactant B is present in far excess of the
stoichiometric requirements for the reaction in the film, then the depletion of the reactant concentration
in the film is negligible. The condition for such a case is given by,
[ ] ( ) [ ] [ ] ( ) * * / * / * *
2
O A O B L O A A
A b D B D K B K D << -- (2)
Where
[ ] *
O
A
is equilibrium concentration of a.
Under such conditions the reaction can be considered to be pseudo first order with respect to the solute
A, and the volumetric rate of absorption of A is given by,
[ ] [ ]
O A O A
B K D A a a R * * * * *
2
-- (3)
from the equation (1) it is clear that the rate of absorption is a unique function of the physico-chemical
properties and completely independent of the hydrodynamics of the system.
The absorption of Carbon dioxide by caustic soda is accompanied by an irreversible chemical reaction
and the partial pressure of CO
2
in equilibrium with the solution is zero. The absorption of CO
2
is
followed by a hydrolysis reaction in solution which can be represented by the equations:
CO
2
+ OH
-
= HCO
3
-
CO
2
+ H
2
O = H
+
+ HCO
3
-
The reaction rate constants determined at 25C are;
Reaction I: k = 2.7710-5 sec
-1
Reaction II: k = 0.0149 sec
-1

The first reaction is operative in the absorption of CO
2
by caustic solutions. Since this is a fast reaction
the factors controlling the absorption are the rates of diffusion of the reactants in the liquid phase. The
second reaction is slow and controls the rate of absorption in carbonate solution. The experimental
results on the absorption of CO
2
by alkaline solutions are usually expressed as the overall gas film
coefficient because the concentration gradient in the liquid is unknown. The results show that the
coefficient K
G
a is inversely proportional to the square root of the absolute gas pressure and tends to
decrease as the packed height is increased The dependence of the coefficient on the gas flow rate is an
indication that at very low concentration the absorption of CO
2
is partially controlled by the gas phase
coefficient. At higher concentration (2% CO
2
) the absorption is wholly controlled by the liquid film.

The effect of temp, NaOH concentration and degree of conversion to sodium carbonate:
The effect of varying the carbon dioxide concentration in gas phase over a range from 3 to 28%, the
overall gas film coefficient, K
G
a, was found to be independent of the gas flow rate, the concentration of
alkali, and the partial pressure of CO
2
in the gas .The experiments of absorption in NaOH solution
showed that K
G
a increased with the normality of the NaOH up to 1.5 N, but was not affected by a further
increase in concentration. The effect of the partial pressure of CO
2
was a function of the normality of the
liquid. At high normality (above 1.5 N), K
G
a decreased as the average partial pressure increased up to a
value of 0.06 atm , but further increase in partial pressure had no effect on the
58
coefficient The coefficient decreased progressively as the sodium hydroxide was converted to carbonate.
The volumetric coefficient, K
G
a appeared to be independent of the packing size
EXPERIMENTAL SETUP:
The equipment consists of one column arranged on the top of the other. Liquid re-distributor and
sampling point (pressure tapping) is provided at the top, bottom of the assembly. Rota meters to measure
the flow rate of Carbon Dioxide, Air and dilute solution of Sodium Hydroxide individually are also
included. The CO
2
is supplied from the cylinder provided and air from the air compressor. Online
mixture is provided for the gases and then they enter the column assembly from the bottom with the help
of gas distributor. The column is filled with Rasching rings of 12 mm size. Aq. NaOH solution is
sprayed with the help of a SS tank, pump, bypass line and pre calibrated Rotameter in counter current
manner to the gas flow. Liquid level adjuster is also provided to ensure liquid seal at the bottom. One
manometer is provided to measure the pressure drop across the columns. The vent of the top column
shall always be kept open. Sample collection bottle is also provided along with it.
PROCEDURE:
Initially start the air compressor and collect sufficient air in the pressure tank so as the pressure is about
3-4 kg/cm
2
. Prepare the dilute NaOH solution in the tank. Open the valve of the pressure tank and allow
the air to pass through the column. Set the air flow at the desired value and then open the valve on the
CO
2
cylinder and adjust the flow rate to predetermined value. Now start the pump for the NaOH solution
and using the bypass valve and feed valve set the desired value of flow rate. After sometime take the
sample at various points (liquid as well as gas) and analyze them.
Initially start the liquid flow at sufficiently high rate (V
L
= 0.03 m/s) to ensure that all the packing are
wetted. The flow rates of gas and liquid are adjusted at predetermined values. The CO
2
flow rate should
be such that the %CO
2
in the mixed gas is about 8-10%. The gas velocity has no effect on the interfacial
area in a packed column. Hence a value of V
G
between 0.1-0.2 m/s may be chosen for all the
experiments and keeping it constant. The linear superficial liquid velocity V is the most important
variable. The range for V should be fixed between 0.001-0.007 m/s.
The system is allowed to reach steady state after fixing the liquid level in the bottom section at a marked
height. Inlet and outlet samples are withdrawn for analysis. This procedure is to be repeated for 6-7
different values of V
L
chosen in such a way that the range indicated is fully covered.
OBSERVATIONS:
System : (CO
2
+Air) + Aq. NaOH solution
Packing Used : Rasching ring of size 12 mm
Column Diameter : mm(ID)
Pressure : k-N/m
2
Packed Height : mm (in each column)
V
G
: m/sec
59
CHEMICAL REACTION:
CO
2
+ NaOH NaHCO
3
NaHCO
3
+ NaOH Na
2
CO
3
+ H
2
O
Final Reaction:
2NaOH + CO
2
Na
2
CO
3
+ H
2
O
Here, NaOH is excess material so stoichiometric reaction is in 2:1 ratio.
Sr.
No.
Flow rate of
Air
LPM
Flow rate of
CO2
LPM
Flow rate of NaOH
Solution
LPM
Burette
Reading
(ml)
1 30 1.58 1 16

The concentration of NaOH used should be between 2-2.5 g mol/lit. The inlet CO
2
percentage is kept
around 10%. Under these conditions the equations (1) and (2) are satisfied and the absorption of CO
2
is
accompanied by a fast pseudo first order.
5 ml of sample (or10 ml) is titrated against standard HCl of molarity (approx.1 g mol/liter) using
phenolphthalein as an indicator.

Titrate Value (V
1
) = ml.
Initially feed of NaOH in g mol/min
Feed normality of NaOH solution is 0.2 N
gm-mol/min = 0.2 g mol/min
After steady state, titrate the product with 0.1 N HCl solution use phenolphthalein as an indicator.
gm-moles of CO
2
in feed = ((flowrate10
-3
density)/Molwt)1000
= ((1.5810
-3
1.5)/44)1000
= 0.05386 gm-moles/min
60
gm-moles of NaOH in feed = Flow rate Normality of feed
= 10.2 = 0.2
Burette reading = 16 ml
So, NaOH consumed = 0.04 gm-moles/min
CO
2
absorbed =0.04gm-moles/min (because stoichiometric ratio is 2:1)

% CO
2
absorbed = (CO
2
reacted/CO
2
in feed) 100
= (0.04/0.0538)100
= 74.5%
RESULT:
Absorption Efficiency of column is 74.5%
CONCLUSION:
By increasing the gas velocity, the rate of absorption and overall efficiency of tower decreases. And vise
versa decreasing gas velocity or increasing liquid flow rate, absorption tower capacity increases. Gas
velocity and liquid flow rate should be in proper range otherwise flooding, channeling can occur.
PRECAUTIONS:
1. Always use clean or distill water for making feed solution.
2. Clean the packed column after conducting the experiment just passing the clean water into it.
3. Drain the column and feed tank of NaOH.
4. Close the CO
2
cylinder after use.
==== X ====
61
Experiment No : 10
BATCH RECTIFICATION IN
A PACKED DISTILLATION COLUMN
62
BATCH RECTIFICATION IN A PACKED DISTILLATION COLUMN
OBJECTIVE:
To study the operation of a packed bed batch rectification column under constant or total reflux
condition.
AIM:
To operate the column under total reflux condition and estimate the minimum number of
theoretical stages required using both Fenskes equation & McCabe -Thieles graphical method.
To estimate the theoretical number of stages at the operating conditions using McCabe
Thieles graphical method.
INTRODUCTION:
Batch distillation is often preferable to continuous distillation in cases where relatively small quantities
of material are to be handled at irregularly scheduled periods. The simplest case of batch distillation is
one in which the material to be separated is charged to a heated kettle, fitted with a total condenser and
product receiver. The material is distilled without reflux until a definite change in composition of still
contents has been effected.
In all types of batch distillation, a quantity of feed is charged to a still pot, or kettle, and heat is applied
to it. The vapor, which is usually passed through a fractioning column, is then condensed, giving the
overhead product while a less volatile residue remains in the kettle at the end of distillation. Continuous
distillation is a steady state process because once equilibrium has been attained, conditions at any given
point remains constant, whereas batch distillation is an unsteady state process, the concentration of the
more volatile component decreasing continually so that the temperature and composition of the mixture
at a point in the system alter as the distillation proceeds.
THEORY:
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 re-boiler, 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:
1 1
1
+
+
+
+
R
x
x
R
R
y
D
n n
(1)
For the binary system:
63
y
2
= 1-y
1
; x
2
= 1- x
1
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
numbers of plates are minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of x
B
and x
D
based on the relative volatility of the components, which is defined in terms of equilibrium
concentrations:

e e
e e
X Y
X Y
2 2
1 1
/
/

(2)
Minimum number of theoretical plates required,
( ) ( ) [ ]
1
log
1 / 1 log
min

D B B D
x x x x
N
(3)
An ideal mixture follows Raoults law, and the relative volatility is the ratio of vapor pressure. Thus,
p
1
= P
*
1
x
1

p
2
= P
*
2
x
2

P
p
y
1
1
(4)

P
p
y
2
2
(5)

2
1
2 2
1 1
'
'
/
/
P
P
x y
x y

(6)
y
1
= p
1
/P (4)
y
2
= p
2
/P (5)
= (y
1
/x
1
)/y
2
/x
2
) = (P
*
1
/P
*
2
) (6)
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.
64
DESCRIPTION OF EXPERIMENT:
The packed column is packed with glass Rasching rings. An electrically heated re-boiler is installed at
the bottom of the column. The bottom product is collected in the tank. The vapors from the top of the
column are condensed in the shell and tube type condenser by circulating cooling water.
A tank with pump and Rotameter is provided for condenser cooling water. The condensate is collected in
reflux drum and feedback to column as reflux and part of it is collected as distillate in product receiving
tank. The complete column is insulated for minimizing the heat loss. Instrumentation is done for
pressure & temperature measurement wherever is necessary.
Condenser
Cold Water Inlet
Automatic
Reflux Rotameter
Devider
Reflux
Distillate
By-pass-valve
X
X
Steam Generator Drain Sump Tank Pump
65

Temperature measurement along the rectification column.
Total No. of Sensors = 6
T1 = bottom temp of column
T2 = bottom temp of column

T3 = Vapor temp.
T4 = Condensate temp.
T5 = Cold water inlet temp.
T6 = Cold water outlet temp.
UTILITIES REQUIRED:
Electricity Supply: 1 phase, 220 V AC, 6.5 kW
Water Supply: 4 LPM (approx.
Refractometer for analysis
REQUIRED CHEMICALS:
Methanol for feed preparation
1. Fill the water in cooling water tank.
1. Fill the re-boiler with a composition of Methanol-water solution (say 50-50%). The total amount
of solution should not be less than 15 liters. The composition of solution should be in the range
of 20 to 70% of methanol by volume.
2. Set a process temperature for the process using the digital temperature controller (DTC). The
temperature range should be in the range 85 to 100C.
3. Start the heaters & cooling water pump.
4. Adjust the cooling water flow rate to a moderate value (say 60 LPH). Never fully close the
bypass valve.
5. Set the cyclic timer for the total reflux.
6. Wait for 25-30 min. for the system to achieve steady state.
66
7. Now take out the samples from the bottom & distillate stream (by closing the timer for short
while).
8. Cool down the samples to room temperature & measure the refractive indices.
10.Now adjust the cyclic timer to a desired reflux ratio & wait for 10-15 min.
11.Now take out the samples from both distillate & bottom product.
12.Cool down the samples & measure their refractive indices.
13.The experiment can be repeated with different set points temperatures & reflux ratios.
Average value of for CH
3
OH-H
2
O system is,
= 3.32
Minimum number of theoretical stages by Fenskes equation:
( )
( )
In
x x
x x
In
N
D B
B D
1
]
1
1
1
min
Also calculate the minimum number of trays using the McCabe- Thieles method.
CALCULATION FOR IDEAL NUMBER OF THEORITICAL STAGES WITH A DESIRED
REFLUX RATIO:
Now reflux ratio is set to R = 0.5
Intercept = x
D
/R+1
Plot the equilibrium curve, and the operating line. Draw the stages as described in McCabe- Thieles
method.

PRECAUTIONS & SUGGESTIONS:
1. Total reflux time should be more than 20 minutes.
2. Dont switch on the heater before filling the feed into it.
3. For condenser the cold water supply should be constant.
4. After the experiment, first close the supply to the heater, wait for 10-15 min, and then close the
water supply to the condenser.
TROUBLE SHOOTING:
In case of any problem regarding operation of the apparatus; the apparatus should be quickly switched
off and electric supply should be cut off.
Electrical:
1. Electric Shock: It means that either earth wire inside the panel is loose or there is no earth
provided in the socket to which the equipment is plugged. So, make it sure that the equipment is
earthed properly.
67
2. Display of 1 on D.T.C./D.T.I. : it means sensors connections are loose. Locate the
point of loose connection and solder it properly.

==== X ====
Experiment No: 11
BATCH RECTIFICATION IN
A SIEVE PLATE COLUMN
68
BINARY DISTILLATION IN A SEIVE PLATE COLUMN
OBJECTIVE:
To analyze the performance of a Laboratory Scale Seive Plate Column. To obtain a desired separation of
an alcohol waste feed product.
AIM:
To operate the column under total reflux condition and estimate the minimum number of
theoretical stages required using both Fenskes equation & McCabe-Thieles graphical method.
To obtain T-x data under total reflux at steady state and compare it with theoretical value.
To estimate the theoretical number of stages at the operating conditions using McCabe-Thieles
graphical method.
INTRODUCTION:
Distillation is the method of separating the components of a solution, which depends upon the
distribution of the substances between a gas and liquid phase, applied to cases where all components are
present in both phases. Instead of introducing a new substance into the mixture in order to provide the
second phase, as is done in gas absorption or desorption, the new phase is created from the original
solution by vaporization or condensation.
The direct separation which is ordinarily possible by distillation, into pure products requiring no further
processing has made this perhaps the most important of all the mass transfer operations.

THEORY:
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 re-boiler, 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:
1 1
1
+
+
+
+
R
x
x
R
R
y
D
n n
(1)
69
For the binary system:
y
2
= 1-y
1
x
2
= 1- x
1
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
numbers of plates are minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of x
B
and x
D
based on the relative volatility of the components, which is defined in terms of equilibrium
concentrations:
e e
e e
x y
x y
2 2
1 1
/
/

(2)
Minimum number of theoretical plates required,
( ) ( ) [ ]
1
log
1 / 1 log
min

D B B D
x x x x
N
(3)
An ideal mixture follows Raoults law, and the relative volatility is the ratio of vapor pressure. Thus,
p
1
= P
1
x
1

p
2
= P
2
x
2
P
p
y
1
1
(4)
P
p
y
2
2
(5)
2
1
2 2
1 1
'
'
/
/
P
P
x y
x y

(6)
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.
DESCRIPTION OF EXPERIMENT:
The column is made of Stainless Steel material with seven plates. An electrically heated re-boiler is
installed at the bottom of the column. The bottom product is collected in the tank. The vapors from the
top of the column are condensed in the shell and tube type condenser by circulating cooling water. A
70
tank with pump and Rota-meter is provided for condenser cooling water. The condensate is
collected in reflux drum and feedback to column as reflux and part of it is collected as distillate in
product receiving tank. The complete column is insulated for minimizing the heat loss. Instrumentation
is done for pressure & temperature measurement wherever is necessary.
Condenser
Cold Water Inlet
Automatic
Reflux Rotameter
Devider
Reflux
Distillate
By-pass-valve
X
X
Steam Generator Drain Sump Tank Pump
Temperature measurement along the rectification column:
Total No. Of Sensors = 11
T
1
= 1
st
Tray temp.
T
2
= 2
nd
Tray temp.
T
3
= 3
rd
Tray temp.
T
4
= 4
th
Tray temp.
71
T
5
= 5
th
Tray temp.
T
6
= 6
th
Tray temp.
T
7
= 7
th
Tray temp.
T
8
= Vapor temp.
T
9
= Condensate temp.
T
10
= Cold water inlet temp.
T
11
= Cold water outlet temp.

UTILITIES REQUIRED:
Electricity Supply: 1 phase, 220 V AC, 6.5 kW
Water Supply: 4 LPM (approx.
Refractometer for analysis
REQUIRED CHEMICALS:
Methanol for feed preparation
1. Fill the water in cooling water tank.
2. Fill the re-boiler with a composition of Methanol-water solution (say 50-50%). The total amount
of solution should not be less than 15 liters. The composition of solution should be in the range
of 20 to 70% of methanol by volume.
3. Set a process temperature for the process using the digital temperature controller (DTC). The
temperature range should be in the range 85 to 100C.
4. Start the heaters & cooling water pump.
5. Adjust the cooling water flow rate to a moderate value (say 60 LPH). Never fully close the
bypass valve.
6. Set the cyclic timer for the total reflux.
7. Wait for 25-30 min. for the system to achieve steady state.
8. Now take out the samples from the bottom & distillate stream (by closing the timer for short
while).
9. Cool down the samples to room temperature & measure the refractive indices.
10. Now adjust the cyclic timer to a desired reflux ratio & wait for 10-15 min.
72
11. Now take out the samples from both distillate & bottom product.
12. Cool down the samples & measure their refractive indices.
13. The experiment can be repeated with different set points temperatures & reflux ratios.
SPECIFICATIONS:
Distillation Column : Material Stainless Steel, Dia 110 mm, Seven trays.
Rotameter : For cooling water flow rate measurement.
Re-boiler : Made of Stainless Steel, (25 Liters) provided with Pressure Gauge, Level
indicator & Safety valve.
Reflux Divider : An electronic cyclic timer is provided to set reflux ratio.
Condenser : Shell & Tube type made of Stainless Steel.
Heater : Nichrome wire heater, 3 kW each, 2 Nos.
Distillate tank : Made of Stainless Steel, capacity 5 Ltrs.

Water supply tank : Made of Stainless Steel, capacity 100 Liters for condenser.
Pump : FHP capacity
Temp. Sensors : RTD PT-100 type
Control panel comprises of :
Digital temp. Controller : 0-199.9C, for re-boiler
Digital Temp. Indicator : 0-199.9C,with multi-channel Switch
With Standard make on/off switch, Mains Indicator etc.
The whole set-up is well designed and arranged in a good quality painted structure.
FORMULAE:
Equilibrium value y corresponding to x can be obtained from:
y
1
= x
1
/(1+(1)x
1
) ; V = D(R+1)
73
( ) ( ) [ ]
1
log
1 / 1 log
min

D B B D
x x x x
N
T-x-y data for Methanol-Water system:
T C x y
100 0 0
96.4 0.02 0.134
93.5 0.04 0.23
91.2 0.06 0.304
89.3 0.08 0.365
87.7 0.1 0.418
84.4 0.15 0.517
81.7 0.2 0.579
78.0 0.3 0.665
75.3 0.4 0.729
73.1 0.5 0.779
71.2 0.6 0.825
69.3 0.7 0.87
67.5 0.8 0.915
66.0 0.9 0.958
65.0 0.95 0.979
64.5 1 1
OBSERVATION & CALCULATIONS:
DATA:
Number of plates = 7
Average value of for Methanol-water system = 3.32
OBSERVATION OF DIFFERENCE IN TRAY COMPOSITION AT OPERATING
CONDITIONS & EQUILIBRIUM COMPOSITIONS:
Steady state tray temperature and composition at total reflux:
Tray No. 1 2 3 4 5 6 7
74
R.I.
Temp.(C)
Values of compositions are found for the respective trays using the calibration curve. These values are
plotted against the respective temp.
SAMPLE CALCULATION FOR MINIMUM NUMBER OF THEORITICAL STAGES:
R-I of Feed = 1.337
R-I of Distillate = 1.344
R-I of Bottoms = 1.345
From the calibration curve, corresponding mole fractions of CH
3
OH is:
x
F
= 0.5
x
D
= 0.72
x
B
= 0.40
Feed Temperature = 21 C

Average value of for CH
3
OH-H
2
O system is
= 3.32
Minimum number of theoretical stages by Fenskes equation:
( )
( )
In
x x
x x
In
N
D B
B D
1
]
1
1
1
min
Also calculate the minimum number of trays using the McCabe- Thieles graphical method.
SAMPLE CALCULATION FOR IDEAL NUMBER OF THEORITICAL STAGES WITH A
DESIRED
REFLUX RATIO:
Now reflux ratio is set to R = 0.5
Intercept = x
D
/R+1
Plot the equilibrium curve, the operating line. Draw the stages as described in McCabe-Thieles method.
75
Number of ideal stages required = N
T
Number of actual stages provided = 7
Overall efficiency of the Seive Plate Distillation Column
At the prevailing operating conditions

= (N
T
/7)100
NOMENCLATURE:
= Relative volatility of the components
= Density
= Time
D = Flow rate of distillate ( moles)
MW = Molecular weight
N
min
= Minimum number of theoretical plates
P = Total pressure
p = Vapor pressure
R = Reflux ratio
V = Vapor flow rate
x = Mole fraction of component in liquid phase
y = Mole fraction of component in vapor phase
SUBSCRIPTS:
1
= First component of binary mixture
2
= Second component of binary mixture
B
= Bottom product (residue)
D
= Distillate
e = Equilibrium
f = Final state
i = Initial state
n = Number of plates
CONCLUSIONS:
PRECAUTIONS & SUGGESTIONS:
1. Heater should not be switched on before charging the solution in still.
2. Always drain tanks and re-boiler when experiment is over.
3. Always use clean water and ensure that there are no foreign particles in the flow stream.
76
==== X ====
77
Experiment No: 12
TO DETERMINE DIFFUSIVITY
COEFFICIENT BY PITOT TUBE
78
PITOT TUBE
AIM:
Calibration of Pitot Tube.
OBJECTIVES
1.) To calibrate a pitot tube.
2.) To determine the pitot co-efficient.
THEORY:
A pitot tube is used to find the velocity of an open stream at any point. The tube bent at its end and
drawn out into a nozzle may be used to find the velocity at point nozzle axis is aligned toward the
direction of flow. The water of stream will rise in the tube at a height equal to stagnation pressure head
which will project out of the free surface by the amount of velocity head. Thus the velocity at tip of
nozzle can be calculated.
V = C
P
/ ) p p ( 2
1 2
= Cp / p 2
P = (P
2
-P
1
) = (
m
-
)*g
6 . 13
m
kg/cm
3

= 1 kg/cm
3
APPARATUS:
Pitot tube, Differential Manometer and Stop watch.
PROCEDURE
1) Start the pump and adjust the flow.
2) Note the initial reading of water H
1
in the tank and collect water for certain timet and note the
reading H
2
calculate discharge Q
act
and mean velocity V
m
.
3) Now take the reading of manometer at different test run.
4) Calculate the velocity at different place.
79
OBSERVATIONS:
Data:
Area of measuring tank a =50*40 =2000cm
3
Dia of pipe = 2.7 cm
Area of pipe(a) =
D
2
/ 4 = 5.72 cm
2
OBSERVATION TABLE
Sr.No. Water Level of
Measuring Tank
Time Volumetric
Flow Rate
Average
Velocity
Manometer
Reading
Initial Final m
3
/sec h1 h2
Plot pressure average velocity vs. pressure drop in a log-log graph paper and determine the value of pitot
co-efficient.
RESULTS:
CONCLUSIONS:
80
Experiment No: 13
STEAM DISTILLATION
81
STEAM DISTILLATION
AIM:

(a) To carry out steam distillation of Acetic Acid from water system.
(b) To compare the experimental results with that theoretically predicted.
INTRODUCTION:
Steam distillation is a unit operation of considerable practical importance. Steam distillation is a term
applied to a distillation process with open steam, i.e., wherein the steam is in direct contact with the
distilling system in either a batch or a continuous operation. Steam distillation has special value where it
is desired to separate substances at a temperature lower than their normal boiling point because of heat
sensitivity or other reasons.
In steam distillation, feeding open steam to a distillation still distills the liquid. The steam carries with it
vapors of volatile liquid and is condensed to separate the liquid from water. Steam distillation is
generally carried out in a cylindrical still with injection of the steam through coils placed in the bottom
of the still with numerous perforations to obtain uniform distribution. The relation between the number
and size of these distributors and pressure drop and rate of flow through them may be determined by
considering the perforations as orifices.
For a binary system, the steam requirement can be calculated from the following equation:
W
B
/W
A
= (101.3-
V
.P
A
) / (
V.
P
A
)(M
B
/M
A
)
Vaporization Efficiency is computed as,
V
= P
A
/P
EXPERIMENTAL SETUP:
The experimental setup consists of 1000 ml three neck round bottom flask with suitable heating mantle
(with regulator to control the temperature, ON/OFF switch and indicator lamp).
Steam necessary for the distillation is generated using a 3000 ml steam generator(inner body SS 304,
outer body Mild steel, and 500 W heater) and is fed to the round bottom flask using a dip pipe. The
vapors generated in the flask are transferred to the condenser using a bend. The condensed vapors are
collected with the help of beaker. The temperature of the flask is measured by using a thermometer. The
entire assembly is supported with the help of a stand.
PROCEDURE:
82
The distillation still is charged with the predetermined volume of A (about 2000 ml).
The steam generator is filled upto75% of its height and the heater is turned on.
Wait till the pressure into the steam generator build up-to nearly 1.5 kg/cm
2
.
Now open only the jacket valve and allow the steam to enter into the jacket to heat the distillation
kettle mixture.
When the temperature in the still reaches 2C below the boiling point determined in first step,
stop the supply of steam in the jacket and the flow of live steam is started through the dip pipe
into the distillation kettle.
The distillation is continued for a sufficient length of time so that about 60-70% of A charged is
distilled.
The distillate collected in the accumulator separates into the organic layer and an aqueous layer.
The two phases are then separately weighted. Similarly the components in the bottoms are
weighted after cooling to room temperature.

wt. of A taken, W
AF
= kg
Wt. of A in the distillate, W
AD
=.k
Wt. of water in distillate, W
BD
=.kg

Wt. of A in bottoms, W
AB
=.kg
Wt. of water in bottoms, W
BB
=.kg
Mol. Wt.of A, M
A
= kg/kg mol

Mol.wt. of B, M
B
=. kg/kg mol
kmol of A in feed N
AF
= W
AF
/M
A
= kmol
kmol of A in distillate N
AD
= W
AD
/M
A
= kmol
kmol of A in bottoms N
AB
= W
AB
/M
A
= kmol
kmol of water in distillate N
BD
= W
BD
/M
B
= kmol
kmol of water in bottoms N
BB
= W
BB
/M
B
= kmol
Material balance for A,
N
AF
= N
AD
+N
AB
83
Steam Distillation Temperature t
b
, =C
Vapor pressure of A at t
b
, P
A
=..kN/m
2
Vapor pressure of B at t
b
, P
B
=..kN/m
2
Partial pressure of A during distillation,
P
A
= 101.3(N
A
/(N
A
+N
B
)) =kN/m
2
Vaporization Efficiency,
V
= P
A
/P
Steam Requirement, W
B
=..
A
B
A V
A V
A
B
M
M
P
p
W
W
*
3 . 101
.. {Ref: B.K Dutta, Principle of Mass transfer

and separation process, pp 351}
Constant boiling temperature = C.
Volume of feed =.m
OBSERVATION TABLE:
Sr.
No.
Time
(Mins.)
Distillate
(ml)
Density
(gm/ml)
Mass
of Distillate (gm)
Burette
Reading
(ml)
DISTILLATE:
SR.
NO.
Normality
Of
Acetic Acid
Grams
Of
A.A.
Moles
of
A.A.
Grams
Of
Water
Moles
Of
Water
Y =
(molesofwater)/
(moles ofA.A.
+Water)
Y
D
(Avg.)
RESIDUE:
SR. Normality Grams Moles Grams Moles X =
84
NO. Of
Acetic Acid
Of
A.A.
Of
A.A.
Of
Water
Of
Water
(molesofwater)/
(molesof A.A.
+Water)
1/
(y-x)

DISTILLATE:
Normality of distillate,

2
1 1
2
*
V
V N
N
=
Moles of A.A. in distillate,
= N*Eq.Weight * volume of distillate collected
=
Molesof A.A. in distillate,
= Mass of A.A.
m.wt.of A.A.
=
Mass of water in distillate,
= Mass of distillate mass of acetic acid
=
Moles of water in distillate,
= Mass of water
m.wt. of water
=
Mole fraction of water in distillate,
y* =. moles of water
moles of(water+A.A.)
=
RESIDUE:
85
Normality of residue,
2
1 1
2
*
V
V N
N

=
Mass of A.A. in residue,
= N * Eq. Weight*Volume of distillate collected
= . gm
Moles of A.A. in residue,
= Mass of A. A.
mol.wt.of A.A.
=
Mass of water in residue,
= mass of residue mass of acetic acid
= . gm
Moles of water in residue,
= mass of water
mol.wt.of water
= . moles
Mole fraction of water in residue,
X
W
=. moles of water
moles of( water+A.A.)
=
GRAPH:
Plot graph 1/(y-x)vs.x.
Find ln F/W that will give the area under the curve where F and W are in moles.
86
The area under the curve obtained beginning at x
F
, when the area equals the
calculated ln F/W, integration is stopped at that point which gives the practical value of x
W
.
From y
D,avg
.find the x
W
using equation: F.x
F
=D.y
D,avg
.+W.x
W

Which will give theoretical value of x
W.
RESULTS:
CONCLUSIONS:
==== X ====
87
Experiment No: 14
ROTARY DRYER
88
ROTARY DRYER
OBJECTIVE:
To study the rate of drying for rotary dryer for different air flow rates and different air inlet
temperatures.
INTRODUCTION:
In many cases, the drying of materials is the final operation in the manufacturing process, carried out
immediately prior to packaging or dispatch. Drying refers to final removal of water, and the operation
then follows evaporation, filtration or crystallization. Drying is carried out for more or more of the
following reasons:
To reduce the transportation cost
To make a material more suitable for handling, for example soap powders, dyestuffs, fertilizers.
To provide definite properties, such as maintaining free flowing nature of salts.
To remove moisture; which may otherwise lead to corrosion, for example, the drying of coal gas
or benzene prior to chlorination.
Almost all drying processes involve the removal of water by vaporization, & thus require the addition of
heat.
THEORY:
Consider a rotary continuous counter-current dryer fed with a nonporous material having all moisture as
unbound moisture. As this material enters the dryer, it is first heated to the drying temperature. It will
then pass through the length of dryer at nearly the wet bulb temperature and theoretically at the end of
the dryer, the material shall be discharged as dry material nearly at the wet bulb temperature.
Assumptions:
No heat losses from the dryer
Heat is applied to the material only from the air, not by conduction from the dryer shell.
All the moisture present is free moisture.
There is no evaporation of moisture in the preliminary heating period.
Drying proceeds at a constant wet bulb temperature until desired amount of water has been removed.
The entering air is assumed at be 100% saturated, so its temperature needs to be raised so as to decrease
the relative saturation. This would enable the air to absorb moisture from the wet solid feed. In turn the
exit air is more saturated than the entering air.
DESCRIPTION:
A rotary dryer consists of a cylindrical shell, set with its axis at a right angle to the horizontal and
mounted on rollers so that it can be rotated. The material to be dried is fed to the high end of the dryer
and by rotation of the dryer, usually assisted by internal shelves of flight, is gradually advanced to the
lower end where it is discharged. The source of heat for a rotary dryer is usually the hot air that
circulates through the dryer. Air flow rate can be measured by the Orificemeter and manometer
provided. Inlet/ Outlet air temperatures (D.B, W.B)are measured by a hygrometer.
UTILITIES REQUIRED:
Electricity Supply: 1 Phase, 220V AC, 4kW
Wet Solid
89
Floor Space of 1.5m 2m
1. Set the preheating temperature of air.
2. Run the blower and note down the wet bulb and dry bulb temperatures of the entering air at the
prevailing temperature.
3. Switch ON the heaters & wait till the set point temperature is arrived.
4. Fill the feed hopper with wet solid.
5. Start the dryer in rotary motion.
6. Allow the wet solid to flow through the dryer by starting the screw conveyor.
7. At steady state record the following:
Air Flow rate( Orifice meter, manometer reading and convert it to volumetric flow rate
and mass flow rate) =G
G
Wet bulb air temperature at outlet = t
w2
Dry bulb temperature at outlet = t
D2
SPECIFICATION:
Drying Shell: Material: SS, Length 1.5m, Dia: 110mm
Feed Hopper: Material: SS, Compatible Capacity
Product Receiver: Material: SS, Compatible Capacity
Rotating Action: Using FHP Crompton/GE make motor coupled with a Reduction Gear Box
Hot Air Circulation: FD Blower fitted with Crompton/GE make motor
Heating Chamber: Fitted with Nichrome wire heater
Air Flow Measurement: Orifice meter and manometer
Control Panel comprises of:
Digital Temperature Controller: 0-200C, RTD PT-100 ype
(For Hot Air)
OBSERVATIONS:
Wet bulb temp. of air at room temp.(C) =
Dry bulb temp. of air at room temp.(C) =
Wet Bulb temperature of
outlet air (C)
Dry Bulb temperature of
outlet air (C)
Manometer Reading
Left Right
FORMULAE AND SAMPLE CALCULATIONS:
Flow Rate of Air:
Manometric difference=h cm
Head in terms of air,
,
_
1
100
air
waer
h
H

90
=
( )( ) ) ( 99 . 9 1
1
1000
100
meter h
h

Diameter of Orifice = 26mm
Diameter of the pipe through which air flows= 52mm
Area of pipe, a
1
= 5.3110
-4
m
2
Area of Orifice, a
2
= 2.12 10
-3
m
2
Flow rate of air,
( )
H g C
a a
a a
Q
d

2
2
1
2
2
2 1
0
= 5.48410
-4
0.614.43H
= 1.48210
-3
H m
3
/sec
Mass flow rate of air = Q
0
= 11.48210
-3
H kg/sec
= 4.68410
-3
h kg/sec
Now, wet air = moisture + dry air
= Y
1
dry air + dry air
= (1+ Y
1
) dry air
Dry air= wet air/(1+ Y
1
)
Mass flow rate of dry air = 4.68410
-3
h/(1+ Y
1
) kg dry air/sec
Where Y
1
= moisture content of air at room temperature
And Y
2
= moisture content of air at outlet during dying
Rate of drying = mass flow rate of dry air (Y
2
-Y
1
)
= 4.68410
-3
h (Y
2
-Y
1
) /(1+ Y
1
) kg moisture/sec
Y
1
and Y
2
are found using the psychrometric chart.
Rate of drying at various flow rates & various inlet temperatures is calculated & graphs between rate of
drying vs flow rate & temperature are plotted.
CONCLUSIONS:
PRECAUTIONS AND MAINTINENCE INSTRUCTIONS:
1. Proper oiling should be necessary for moving parts like roller.
2. Feed should be in granular.
3. Before switching on heaters; switch the blower ON.
==== X ====
91
Experiment No : 15
FORCED DRAFT TRAY DRYER
92
FORCED DRAFT TRAY DRYER
OBJECTIVE:
Drying of solids in a tray dryer under forced draft tray condition.
AIM:
To determine the drying rate of a solid under forced draft condition and determine the critical moisture
content.
INTRODUCTION:
In many cases, drying of materials is the final operation in the manufacturing process, carried out
immediately prior to packaging or dispatch. Drying refers to the final removal of water, and the
operation often follows evaporation, filtration or crystallization. Drying is carried out for one or more of
the following reason:
To reduce the cost of transport.
To make a material more suitable for handling.
To provide definite properties.
To remove moisture this may otherwise lead to corrosion.
THEORY:
Drying of solids is considered to occur in two stages, a constant rate period followed by a falling rate
period. In the constant rate period, the rate of drying corresponds to the removal of water from the
surface of the solid. The falling rate period corresponds to the removal of water from the interior of the
solid. The rate in either case is dependent on:
1. Flow rate of air.
2. The solid characteristics.
3. Tray material.
The rate of drying can be determined for a sample of substance by suspending it over an electronic
balance in the duct, in a stream of air, from a balance. The weight of the drying sample can then be
measured as a function of time. Certain precautions must be observed if the data are to be of maximum
utility. The sample should not be too small. Further, the following conditions should resemble as closely
as possible those expected to prevail in the contemplated large-scale operation:
(I) The sample should be similarly supported in a tray or frame.
(II) It should have the same ratio of drying to non-drying surface.
(III) It should be subjected to similar conditions of radiant heat transfer; and
(IV) The air should have the same temperature, humidity and velocity( both speed and direction
with respect to the sample).
If possible, several tests should be made on samples of different thicknesses. The dry weight of the
sample should also be obtained. The drying rate is calculated from:
93
( ) s m kg
A d
dx
S N
2
/
1
.
DESCRIPTION:
A schematic diagram of the experimental set-up is given below:
AIR IN AIR
OUT
TRAY
It is a wind-tunnel type tray dryer. The main components are;
Drying chamber
Air blower
Heater
Orifice in the air duct
A tray
Balance
The air flow is controlled by a valve in the blower outlet and its flow rate is measured by a pre-calibrated
orifice meter. Thermometers are placed at the inlet and outlet of the drying chamber.
UTILITIES REQUIRED:
Electricity Supply: 1 Phase, 220V A.C, 2.5kW
Wet Solid
Floor area 0.75m 2m
1. Load the pre-weighed tray with solid and record the weight of sand & tray.
2. Start the blower and heater. Fix the air flow rate and let the system to achieve steady state as the
air flow rate would make the temperature steady.
3. When the desired conditions of temperature and air velocity are reached( in about 10-15min),
remove the sample tray and put known amount of water in it to give desired initial moisture
content.
4. Place the tray gently in the drying chamber and start the stopwatch.
5. Record the balance reading with time at about 3-5min time interval.
6. Drying is assumed to be complete when at least 3 consecutive readings are unchanged.
7. The temperatures at the inlet and outlet of the drying chamber and the air flow rate( manometer
reading fixed across the orifice) are recorded at least three times during the course of run to give
average operating conditions.
8. The same steps are repeated for other runs at different operating conditions.
94
The range of variables may be fixed as given below:
Air Flow rate = 8 to 10 cm manometric difference
(with water as manometric fluid)
Initial Moisture Content = 20-50% (Prepare the sample in this range of moisture content)
SPECIFICATION:
Drying Chamber : Insulated double wall chamber. Size:8810
Weighing Balance : Digital, 0-1000gm of 1 gm resolution.
Hot Air Circulation : Blower fitted with Crompton/GE make FHP motor
Heating chamber : Nichrome wire heater of compatible capacity.
Air flow measurement : Orificemeter & manometer.
Control Panel comprises of
Standard make on/off switch, Mains Indicator etc.
FORMULAE:
Moisture content present in solid, X(kg water/kg dry solid)
X = (W-S)/S
The drying rate is thus calculated from:
,
_

s m
kg
A d
dx
S N
2
1

X
A
S
N
Tray diameter = 150mm
Surface Area of Solid = 0.0706m2
Solid dry wt. =
Initial moisture content =
Manometric difference, R = m
,
_
1
a
m
R h
Superficial air flow rate G =

s m
kg
gh a
a

2 0
2 61 . 0
S. No. Time, sec Wt. of solid
(solid + water),kg
X=(W-S)/S (kg
water/kg dry solid)

X
A
S
N
95
Plot X Vs and draw a straight line through all points. Fit a second degree polynomial to the X Vs
data and obtain the slope dX/d corresponding to various values of
The drying rate is thus calculated from:
,
_

s m
kg
A d
dx
S N
2
1

X
A
S
N
Plot drying rate N (kg/m
2
-s)Vs moisture content X (kg of water/kg of dry solid). From this plot
critical moisture content (X
c
) can be obtained.
The experiment can be repeated at constant air flow rate and constant air temperature.
CONCLUSIONS:
NOMENCLATURE:
A = Dying surface area, m
2
G = mass velocity of gas, kg/m
2
-s
N = drying rate, kg/m
2
-s
N
c
= constant drying rate, kg/m
2
-s
S = mass of dry solid, kg
T
g
= absolute temp. of gas (dry bulb), K
X = moisture content of solid (kg of water/kg of dry solid)
= time, sec
= density, kg/m
3
m
= density of manometric fluid, kg/m
3

a
= density of air, kg/m
3
a
0
= area of orifice, m
2
W = mass of wet solid, kg
PRECAUTIONS AND MAINTAINENCE INSTRUCTION:
1. Dont open the door of the chamber during experiment.
2. Dont disturb the balance during experiment.
3. Never switch on heaters before blower.
==== X ====
96
Experiment No : 16
HUMIDIFICATION-DEHUMIDIFICATION
COLUMN
(Evaluation of Mass Transfer Co-efficient)
97
HUMIDIFICATION-DEHUMIDIFICATION COLUMN
(Evaluation of Mass Transfer Co-efficient)
AIM:
To calculate the mass transfer coefficient in the Humidification and Dehumidification column.

THEORY:
In the processing of materials it is often necessary either to increase the amount of vapor present in a gas
stream, an operation known as humidification; or to reduce the vapor present, a process referred to as
dehumidification. In humidification, the vapor content may be increased by passing the gas over a liquid
which then evaporates into the gas stream. This transfer into the main stream take place by diffusion, and
the interface simultaneous heat and mass transfer take place according to the system. The reverse
operation is called dehumidification. The most widespread application of humidification and
dehumidification involves the air-water system. Drying of wet solids is an example of humidification.
The mass transfer coefficient, Ka, can be measured in a humidification and dehumidification column in
which area of contact between two phases is known and boundary layer separation does not take place.
A humidification and dehumidification column also provides useful information on mass transfer to and
from fluids in turbulent flow.
Method of increasing humidity:
Water is sprayed into the gas at such a rate that on complete vaporization it gives the required humidity.
In this case the temperature of the gas will fall as the latent heat of vaporization must be supplied from
the sensible heat of the gas and liquid.
Method of decreasing the humidity:
Dehumidification of air can be effected by bringing it into contact with a cold surface, either liquid or
solid. If the temperature of the surface is lower than the dew point of the gas, condensation takes place
and the temperature of the gas falls. The temperature and humidity are reduced simultaneously
throughout the whole process.
A humidification column is essentially a vertical tube with means of admitting liquid at the top and
causing it to flow downward along the inside wall of the tube, under the influence of gravity and means
of admitting gas to the inside of the tube, where it flows through the tower in contact with the liquid. In
absence of ripple formation at the liquid surface, the interfacial area, A, is known and form drag is
absent.
Various dimensionless groups that control the phenomenon are:
Reynolds Number, N
Re
= dG/
Schimidt Number, N
Sc
= /D
Sherwood Number, N
Sh
= kd/D
G = Gas mass velocity, kg/m
2
s
D = diffusivity coefficient, m
2
/s
D = tube diameter, m
Ka = mass transfer coefficient
98
For turbulent flow mass transfer to pipe involving evaporation of liquids in wetted wall
towers, Gilland and Sherwood proposed the correlation:
44 . 0 81 . 0
Re
023 . 0
Sc Sh
N N N (1)
for
3500 2000
Re
N

5 . 2 6 . 0
Sc
N
atm P 3 1 . 0
The known flow rate of air at a measured humidity is brought into contact with a film of water at a
certain temperature and vapor pressure. Moisture is absorbed be the air from water film and the resultant
humidity of the exit air and the temperature and vapor pressure of the entry water measured. The rate of
diffusion through the gas film, N
A
, is given by:
N
A
, kgmol/h = Ka A (P)
m
(2)
Ka = gas film coefficient, kgmole of water transferred.m
2
/h per atmospheric partial pressure difference.
A = Wetted surface of column = dL
(P)
m
= Log mean partial pressure driving force across the ends of the column.
The value of Ka obtained experimentally can be compared with that predicted from Sherwood
Gilleland correlation:
44 . 0 8 . 0
.
. .
.
.
,
_
,
_
,
_
d
V d
T R
d D
K
a
(3)
d= Column diameter.
DESCRIPTION:
The setup consists of two glass columns with packings of raschig ring and silica gel. Air flow rates can
be set and measured by Rotameter and temperature by RTD. The setup studies are in volumetric mass
transfer coefficient.
FEAUTRES:
(1) Compact Model.
(2) Safe Operation.
(3) Digital Temperature Indication.
In this system the air is firstly free from moisture by passing in the heated chamber and then inserted in
the column from the bottom and water is from the top and comes down with the packing wall. The
moisture is absorbed from the glass column and goes up in the cooling chamber for dehumidification and
then passed into the silica gel filled glass column for complete dehumidification and then passed into the
atmosphere. Water is recycled in the sump tank through the pump. The temperature of the air dry bulb
and wet bulb are measured by RTD 100 provided.
UTILITIES REQUIRED:
99
Compressed Air Supply at 2 Bar, 4 CFM
Water Supply
Drain
Electricity Supply : 1 Phase, 220V AC, 0.5kW
1. Fill the sump tank with water and also connect the air supply to the point provided.
2. Connect the plug to mains and start heating the chamber and also start the air and maintain air
flow rate.
3. Fill the wet bulb thermometer bottle with water and wait for 30 minutes and control the air
temperature by regulating the voltage variac provided.
4. Commence the operation with minimum airflow and after 15-20 minutes, the humidity of inlet
air and the outlet air at this flow rate of air is noted and read corresponding vapor partial
pressure, from the psychometric chart. Simultaneously the temperature of the water in and out is
noted and flow rates are measured. From Steam tables obtain vapor pressure of water
corresponding to these temperatures.
5. Repeat step 3 for 3-4 air flow rates.
6. Calculate experimental value of Ka using equation (2)
7. Calculate the predicted value of Ka using equation (3)
8. Compare the experimental and predicted value of Ka
9. Plot
Re
44 . 0
VsN
N
N
Sc
Sh
on log-log scale and check the slope approximates to 0.8.
SPECIFICATION:
Column = 50mm diameter 500mm height
Shell and Tube Condenser = 114mm diameter 500mm S.S
Tanks = 25 Lit S.S (2 NO.)
Heater Box = 2 kW
Pump = FHP
Compressor required = 1 CFM
Temperature measurement = RTD
Air Flow measurement = Rotameter
Humidification measurement = Wet and Dry Bulb
Control Panel = Electrical
Structure = M.S
Space = 1000L 500W 1500H
Utilities required = 230V, AC
FORMULAE:
Humidity =
( )
O H T
O H
p p
p
2
2
29
18
From steam tables, corresponding to water inlet and outlet temperature calculate the vapor pressure.
100
Calculate (P)
m
as:
(P)
m
=
,
_
B
B
B B
p
p
p p
1
1
ln
where p
B1
= (p
T
p
a1
)
and p
B
= (p
T
p
a
)
OBSERVATIONS & CALCULATIONS:
Column diameter = d
Effective Column Height = L
Room Temperature
Atmospheric Pressure (Total Pressure) = p
T
Surface Area = dL
OBSERVATION TABLE:
S.No Air Temperature C Water Temperature
C
Humidity
In Out In Out Inlet Outlet
Dry
Bulb
Wet
Bulb
Dry
Bulb
Wet Bulb
From Psychometric chart
Note inlet and outlet humidity of air
- Calculate N
A
- Calculate air partial pressures from:
Humidity =
( )
O H T
O H
p p
p
2
2
29
18
From steam tables, corresponding to water inlet and outlet temperature calculate the vapor pressure.
Calculate (P)
m
as:
,
_

B
B
B B
m
p
p
p p
P
1
1
ln
where p
B1
= (p
T
-p
a1
)
and p
B
= (p
T
-p
a
)
101
p
a1
= partial pressure of diffusing component, a, at the boundary
pa = mean value of partial pressure of component, a, in the flowing stream
D for air at 40C = 0.288cm
2
/sec
Calculate Ka
Plot
Re
44 . 0
vsN
N
N
Sc
sh
on log-log scale and determine the slope and intercept.
CONCLUSIONS:
PRECAUTIONS AND MAINTAINENCE INSTRUCTIONS:
1. For condenser the cold water supply should be constant.
2. Dont switch on the pump at low voltage.
3. Air should be moisture free.
4. Wet bulb temperature should be properly contacted with water.
TROUBLESHOOTING:
1. If any type of suspended particle come in the Rotameter, remove the rotameter, clean it and then
fit it.
2. If there is any leakage, tight that part or remove that and refix that again after wrapping Teflon
tape.
3. If Rotameters fluctuating more than average tight control knob of that.
( Procedure: Two nuts are there loose first nut and tight the second slightly, and then first also.
Both nuts are on Rotameters)
5. If switch ON the heater but temperature cant rise but panel LED is ON it means bath heater had
==== X ====
102
Experiment No : 17
LIQUID-LIQUID EXTRACTION IN
A SPRAY COLUMN
103
LIQUID-LIQUID EXTRACTION IN A SPRAY COLUMN
OBJECTIVE:
Study of Extraction in a Spray Column.
AIM:
To study the effect of dispersed phase flow rate on:-
1) Over all volumetric mass transfer coefficient, K
La
2) Dispersed phase hold up.
INTRODUCTION:
Liquid Extraction sometimes called solvent extraction is the separation of the constituents of a liquid
solution by contact with another insoluble liquid. If the substances constituting the original solution
disturb themselves differently between the two liquid phases, a certain degree of separation will result &
this can be enhanced by use of multiple contacts. Spray column involves the dispersion of one of the
liquids involved in liquid- liquid extraction. Usually the liquid with largest volume rate is dispersed
giving largest interfacial surface for a given drop size. Also, the dispersed phase should not wet the
material of the nozzle.
THEORY:
A Spray column may be operated as continuous counter current extraction equipment wherein one of the
liquids forms the dispersed phase, or in semibatch operation, where the continuous phase has zero
velocity. However, in such columns, the back-mixing in continuous phase decreases the driving force for
mass transfer. As a result, the spray columns have low extraction efficiency. The height of a transfer unit
is more as compared to other extraction equipments. Usually the spray columns are used for systems
where number of transfer units is less than five.
At flow rates below those causing flooding, the ratio of slip velocity (V
s
) to the terminal velocity of a
single particle in a quiescent fluid, is a unique function of dispersed phase hold-up for all vertically
moving fluid particle systems. Slip velocity is the net linear velocity between the dispersed phase liquid
and the continuous phase liquid.
Thus in a counter current spray column
d
c
d
d
s
V V
V

+
1
(1)
where V
c
and V
d
are the superficial velocities of the continuous and dispersed phase liquids respectively.
V
d
=
2
3
2
4
m
s
m
D
F
c
D
(2)
D
c
= Column I.D (m)
F
D
= Volumetric flow rate of dispersed phase, m
3
/s
104
d
= Fractional hold up the dispersed phase
(Hold up of dispersed phase)/(Effective volume of column, V

e
) (3)
V
e
= Volume of continuous phase liquid taken in the column.
At the flooding condition, the hold-up is best established by a characteristic velocity of the droplet V
k
,
given by
d
c
d
d
s
V V
V

+
1
= V
k
(1-
d
) (4)
If the superficial velocity of the continuous liquid phase is zero.
0
c
V
( )
d d k d
V V 1
(5)
Thus a plot of V
d
Vs
d
(1-
d
) should yield a straight line through (0,0) with slope V
k
Consider a quiescent continuous liquid phase (Toluene) with Benzoic acid dissolved in it, having an
initial conc. of C
Ti
, kmol/m
3
; using pure water as dispersed phase.
Let C
i
be the initial conc. of Benzoic acid in inlet water (kmol/m
3
)
C
0
be the conc. of Benzoic acid in outlet water (kmol/m
3
)
C* be the equilibrium conc. of Benzoic acid.
Defining log mean conc. difference (driving force) as
( ) ( )
( ) ( ) [ ]
0
0
ln
* * ln
* *
C C C C
C C C C
C
i
i

(6)
C
i
= 0 for pure water.
Dispersed
Phase C
i
Continuous Phase
Interface
Volumetric rate of extraction of Benzoic Acid, kmole/m
3
-s = R
A
a
Volumetric rate of extraction of Benzoic acid, kmol/m

3
-s = R
A
a
105
e
d
A
V
F C
a R
0
(7)
or Rate of mass transfer ( ) h gmol F C C
N
d i a
/ ,
Overall Volumetric mass transfer coefficient (1/s) is thus defined as:

( )
ln
C
a R
a K
A
L
(8)
A plot of K
L
a Vs V
d
on a log-log scale indicates the effect of dispersed phase liquid velocity on the M.T
Coefficient (K
L
a)
DESCRIPTION:
The present set up is shown for semi-batch operation, though same set up can be used for continuous
operation as well as by allowing the continuous phase liquid to flow at a low flow rate.
The dispersed phase liquid (water) is metered through a pre-calibrated Rotameter. In case of continuous
operation, the continuous phase liquid (Toluene) can also be metered through another pre-calibrated
Rotameter provided with the setup. The liquid-liquid interface is maintained at a suitable height from the
bottom by adjusting the extract flow rate at the bottom. This is done by adjusting the height of the
flexible pipe provided at the bottom outlet of the dispersed phase liquid.
UTILITIES REQUIRED:
Compressed Air Supply at 2 Bar, 0.5 CFM
Water Supply.
Drain
Required Chemicals & Laboratory Glassware.
1. Prepare a solution of Toluene+Benzoic Acid by dissolving Benzoic Acid in Toluene such that the
conc. of Benzoic Acid in Toluene is = 0.2gmole/L or 0.2kgmole/m
3
2. Fill the spray extraction column with Toluene containing Benzoic Acid to such a height that the
dispersed phase nozzle just dips in the pool of Toluene.
3. Adjust the Rotameter reading for water (dispersed phase) to a prefixed value (4LPH to 15LPH)
4. Adjust the outflow from the column such that the liquid-liquid interface is maintained at a
suitable height from the bottom. Maintain the interface at the same height for all observations.
Record the volumetric flow rate of water (F
d
)
5. Collect 40ml of water sample at the outlet stream of the column after 10 to 15 minutes of
operation (S.S condition). Since the continuous phase is already saturated w.r.t the dispersed
phase, the direction of mass transfer, therefore is only from continuous phase to the dispersed
106
phase. Titrate the sample with N/10 or N/20 NaOH using Phenolphthalein as
indicator and determine the conc. of Benzoic Acid in water at the outlet (C
0
)
6. Close the inlet and outlet to the column simultaneously and allow the dispersed phase droplets to
coalesce and settle.
7. Collect the hold up until the interface drops to the initial height from the bottom. Measure the
volume of the hold up.
8. Repeat the above steps for at least four different values if dispersed flow rates.
SPECIFICATION:
Extraction Column = Material Borosilicate Glass
Dia. 45mm, Height 750mm (approx)
Feed Tank = Material SS, Capacity 20 Ltrs, 2 No.s
Extract and Raffinate Tanks = Material SS, Capacity 10 Ltrs, 2 No.s
Piping = SS and PVC, Size
Feed Circulation = By compressed air
Pressure Regulator = 0-2 kg/cm
2
Pressure Gauge = Bourdan type, 0-2 kg/cm
2
Flow Measurement = Rotamaters (One each for Solvent & Solute)
FORMUILAE:
Dispersed phase superficial velocity = V
d
=
) / ( h m
A
F
c
D
Fractional Hold up =
d
=
( )
( ) L V
L V
e
w
3
10
Conc. of Benzoic Acid in water at the outlet :

(V
1
N
1
)
Benzoic Acid
= (V
2
1/10)
NaOH
40N
1
= V
2
1/10
L gmole L gmeq
V
N / /
400
2
1

= kmole/m
3
= C
i
From the equilibrium data of Toluene-Benzoic Acid-water
(Ref. I-E-C 29,451(1937))
C*
w
/C
T
= 0.167267-0.837941C
T
+2.27418C
T
2
For C
T
= 0.2 gmol/L
C
w
/C
T
= 0.090646 = m
107
Considering C
T1
= C
T2
= C
T
= 0.2 gmol/L
C
w1
= 0
C
1
= C
T1
C
w1
/m = C
T1
C
i
/m
C
2
= C
T2
C
w2
/m = C
T2
C
0
/m
( ) ( )
( ) ( ) [ ]
0
0
ln
* * ln
* *
C C C C
C C C C
C
i
i

Rate of mass transfer = N/ = C
0
F
D
Effective Volume of Toluene = V

e
(L)
M.T Coefficient = K
L
a =
( )
ln
C V
N
e

( )
h m
V
V
d d
d
k
/
1
OBSERVATION AND CALCULATION:

Temperature =
Volume of sample for each titration = 40 ml
Run
No.
Water Flow rate (F
d
), LPH Hold up collected V
w
,
ml
Vol. of N/10 NaOH used for
titration (V
2
), ml
CALCULATIONS:
I.D of column = D
c
(m)
Effective volume of Toluene in the column = V
e
(ml)
Conc. of BA in Toluene, C
T
= 0.2 kmol/m
3
Cross sectional area of column = A
c
= ( )
2 2
4
m D
c
Dispersed phase superficial velocity, V

d
=
h m
A
F
C
D
/
Fractional Hold up,
d
=
( )
( ) L V
L V
e
w
3
10

108
Conc. of Benzoic Acid in water at the outlet :
(V
1
N
1
)
Benzoic Acid
= (V
2
1/10)
NaOH
40N
1
= V
2
1/10
L gmole L gmeq
V
N / /
400
2
1

= C
i
kmole/m
3
(Ref. I-E-C 29,451(1937))
C*
w
/C
T
= 0.167267-0.837941C
T
+2.27418C
T
2
For C
T
= 0.2 gmol/L
C
w
/C
T
= 0.090646m
Considering C
T1
= C
T2
= C
T
= 0.2 gmol/L
C
w1
= 0
C
1
= C
T1
C
w1
/m = C
T1
C
i
/m
C
2
= C
T2
C
w2
/m = C
T2
C
0
/m
( )
1
]
1

2
1
2 1
ln
ln
C
C
C C
C
Rate of mass transfer = N/ = C
0
F
D
Effective Volume of Toluene = V

e
(L)
M.T Coefficient = K
L
a =
( )
ln
C V
N
e

( )
h m
V
V
d d
d
k
/
1
OBSERVATION TABLE:
R. No. V
d
(m/h) Q
d
F
d
(LPH) (c)
ln
,
gmol/L
R
A
a
gmole/m
3
h
Q
d
(1- Q
d
) K
L
a L
-1
109
Plot V
d
Vs
d
(1-
d
), draw a straight line through (0,0) and obtain the slope V
k.
Plot K
L
a Vs V
d
on a log-log scale
Discuss your results.
CONCLUSIONS:
NOMENCLATURE:
D
c
= Column I.D (m)
F
D
= Volumetric flow rate of dispersed phase liquid, m
3
/s
d
= Fractional hold up of the dispersed phase
K
L
a = M.T Coefficient
V
e
= Effective volume of Toluene
A
c
= Cross sectional area of column
C* = Equilibrium conc. of Benzoic Acid
C
T
= Conc. of B.A in Toluene.
C
w
= Conc. of B.A in water.
V
d
= Dispersed phase superficial velocity
N/ = Rate of mass transfer.
PRECAUTIONS & MAINTAINENCE:
1. Prepare the feed solution in exactly as per our manuals.
2. Make the interface always 1 inch above the water inlet sparger.
3. Interface should not be disturbed.
4. Feed tank should be clean.
5. Always use clean water.
6. Dont exceed the flow rate at 15LPH
7. Water outlet should be toluene free.
TROUBLESHOOTING:
1. If any type of suspended particles come in the Rotameter, remove the rotameter clean the tube
and fit it at its place.
2. If there is any leakage, tight that part or remove that and refix again after wrapping Teflon tape.
3. If Rotameter fluctuates more than the average tight control knob of that.
(Procedure: Two nuts are there lose first nut and tight the second slightly, and then first also.
Both nuts are on rotameter.)
==== X ====
110
Experiment No : 18
SOLID-LIQUID EXTRACTION UNIT
(BONNOTTO TYPE)
111
SOLID-LIQUID EXTRACTION UNIT
(BONNOTTO TYPE)
OBJECTIVE:
Study of Solid Liquid Extraction in a Column with Solid in Batch & Liquid in Continuous Recirculation.
AIM:
To study the effect of various system parameters like: solvent temperature, solvent rate and particle size
on the % recovery of oil from oil seeds.
INTRODUCTION:
Leaching is a method of extracting a desired chemical that is dispersed or dissolved in a solid. The solid
is ground up into small pieces and washed with a solvent in which the desired chemical is soluble.
Sometimes the solid and solvent from slurry that can be conveyed. In any event the desired chemical is
transferred from the solid to the liquid phase. The resultant liquid, which is rich in the desired chemical,
is filtered to remove fine suspended grains of the solid. The liquid can then be distilled or otherwise
purified.
THEORY:
Leaching is a common industrial process, but it also occurs in natural systems, such as in the motion of
water through soil. In this case, the solid phase is soil particles, and the leaching solvent is water,
presumably rain water that percolates through the soil. Some chemicals attached to the soil particles are
water-soluble. These chemicals are transferred to the water as it flows through the soil. Such a process
sometimes called in-situ leaching, because it occurs with the solid phase fixed in place.
The laboratory experiment uses simple equipment to explore a leaching operation that is familiar to all of
usthe extraction of oil from oil seeds using hexane as the leaching solvent.
DISCUSSION:
Oil seeds contain edible oil in it. When oil seeds are mixed with hexane oil, oil is transferred from the
solid oil seeds. The rate of mass transfer and, therefore, the concentration of the oil in the hexane phase,
are strongly affected by several variables. We will examine quantitatively a few of the variables that
affect the leaching process.
Oil seed is placed inside a glass column in the form of a packed bed. Hot or cold hexane flows up the
packed bed, extracting the oil that is present in the seeds. The concentration of the oil probably depends
upon many variables, like: the amount of oil seed in the bed, the volume of hexane used, temperature of
hexane and the coarseness of the solid oil seeds.
UTILITIES REQUIRED:
Electricity Supply : 1 Phase, 220V AC, 3kW
Hexane : 50 Ltrs
Oil seeds : 30kg
112
PROCEDURE:
1. Fill the glass column with the known weight of air-dried oil seeds (W
0
), gms, the initial amount of
oil present in the dried oil seeds must be known (x
0
), gm of oil/gm of seed..
2 Fill the solvent feed tank with hexane. Select a suitable operating temperature (25 to 45C) and heat
the hexane to this temperature.
3. Allow the hot hexane to enter the packed bed slowly and return the solvent to the feed tank i.e the
operating process shall be in a closed cycle.
4. Note the flow rate of hexane and run the experiment for 3 hours. After 3 hours, stop the solvent
supply and remove the wet seeds from the column in an open tray. Dry the material first in open air
then in an oven till constant weight.
6. Weigh the dry seeds. Let the weight of dry seeds=W, gm
7. Oil extracted = O
e
=( W
0
- W), gm
8. Max. oil present in seeds = O
max
= W
0
x
0
, gm
9. % recovery= (O
e
/ O
max
)100
The experiment can be repeated for:
Different solvent temperatures.
Different oil seed sizes (or bed porosity)
Different solvent rates
Discuss your results.
SPECIFICATIONS:
Extraction Column : Material SS, Dia 150mm, Height 750mm (approx)
Plates : Material SS, with radial opening
Mixer : SS Impellers fitted on SS shaft coupled to a Crompton / GE make
motor and reduction gear box.
Screw Conveyor : Material SS, Compatible capacity, housed in GI pipe and driven by a
Crompton / GE make motor and reduction gear box.
Solvent Flow measurement : Rotameter
Solvent Tank : made of SS, Capacity 30 Ltrs. Double wall
Feed Circulation : Magnetic Pump made of Polypropylene to circulate solvent. Maximum
working temperature is 60C.
Heater : 1.5 kW Nichrome Wire Heater.
Feed Hopper : Suitable capacity
Filtration Sieve : Material SS, Compatible capacity
Receiving tank for : Material SS, Compatible capacity
Extracting solid waste
Control Panel comprising of :
Digital Temp. Controller 0-200C, RTD PT-100 type
(For feed tank)
Standard make on/off switch, Mains Indicator etc.
113
A good quality painted rigid MS structure is provided to support all the parts.
OBSERVATIONS & CALCULATIONS:
DATA:
Column diameter:
Packed Height:
Bed Porosity:
Oil seed size:
Solvent:
Solvent rate:
Solvent temperature:
Wt. of air dried seeds in the packed bed = W
0
gm
Initial conc. of oil in oil seeds = X
0
, gm of oil/gm of seed
Run time =
Wt. of exhausted oil seeds (dried to constant wt.) = W, gm
Oil recovered : O
e
gm = ( W
0
- W), gm
Max. oil content in oil seed = O
max
, gm = W
0
x
0
, gm
% Oil Recovery = (O
e
/ O
max
)100
Compare the % recovery for different parameters under which the leaching was carried and discuss your
results.
CONCLUSIONS:
NOMENCLATURE:
W
0
= Wt. of air dried seeds in the packed bed
X
0
= Initial conc. of oil in oil seeds
W = Wt. of exhausted oil seeds (dried to constant wt.)
O
e
= Oil recovered
O
max
= Max. oil content in oil seed
PRECAUTIONS & MAINTINENECE INSTRUCTIONS:
1. Always use fresh oil seed or expeller waste that should be some oil.
2. Hexane should be oil free or not used.
3. Dont switch on the heater before filling the water in the bath.
4. Proper cleaning should be necessary for the set-up.
114
==== X ====
115

Experiment No : 19
FLUIDIZED BED DRYER
116
FLUIDIZED BED DRYER
AIM:
To plot the drying curve under fluidized bed condition.
THEORY:
Granular solids fluidized by a drying medium such as hot air, can be dried and cooled in a fluidized bed.
The principal characteristics of such beds include cross flow of solid and drying gas, a solid residence
time controllable from seconds to hours and suitably for any gas temperature. It is necessary that solids
be free flowing and of a size range 1mm to 2mm. Since the mass flow rate of gas for thermal
requirements is substantially less than that required for fluidization, the bed is most economically
operated at the minimum velocity for fluidization.
During fluidization the particles are circulated within the fluidized bed. This circulation has a direct
bearing on the heat transfer properties of gas solid fluidized bed systems. Fluidized beds have been used
for heat exchange in both physical operations and chemical processes because of rapid transport. Also
because of mixing, uniform temperatures throughout the bed can be maintained.
CALCULATION OF DRYING CURVE FROM THE RECORD OF MOISTURE CONTENT OF THE
DRYING MEDIUM.
If a sample of wet material containing Z
0
kg of dry material, is dried at a constant flow rate of air, L
0
kg
of dry air per hour, whose initial humidity is x, the time dependence of moisture content of the sample,
can be determined from the changes in humidity of the drying medium, x = xx, where x is the final
moisture content of the drying medium.
The differential moisture balance is:

x
Z
L
dt
dc

0
0
(1)
On integration this equation yields:

t
xdt
Z
L
c
0 0
0
(2)
c
0
= Initial moisture content of the material
c = Moisture content of the material at any time t, (gm of water / gm of dry solid) 100
The value of the integral can be determined graphically.
From the course of x, time dependence of the fraction of water evaporated and can be calculated
from:
117
0
0
xdt
xdt
t
(3)
Then c= c
0
-[c
0
-c] (4)
Where c
= c at t
In some cases, the change in the humidity of the drying air, x, on passing through the dryer is small the
calculation of the drying curve ( vs t) from eq. (2) is insufficiently accurate.
In case, we record the variation in moisture content of the material(c) with time, t, the eq. (4) can be used
to construct the dying curve.
c c
c c
0
0
= fraction of water removed from the material.

c
0
= Initial moisture content of the material,
100
solid dry of gm
moisture of gm
= % moisture based on dry wt.

c
= final equilibrium moisture content ( at t )

c= Instantaneous moisture content ( at t = t)
DESCRIPTION:
The set up consists of a
Glass column, the conical
portion of which is filled
with fluidizing material.
The material is supported
on the screen mesh held
between two flanges. Air
from the compressor is
heated in the heater box
and passed through the
column. Air rotameter is
provided to measure the
air flow rate. The flow rate
can be adjusted by SS
needle valve provided for
air supply to the column.
A thermocouple is
provided for the
measurement of
temperature of air at the
inlet of the column at
bottom.
Cyclone
105 mm
200 mm
Wet
material
T
118
Hot
Air
FIGURE - 1
UTILITIES REQUIRED:
1. Overall Space = 2m L 2m W 2m Ht
2. Fluidizing material = Silica sand of size < 2mm. Qty approx 200
3. Electricity = 1 Phase, 230V AC, 3kW
4. Compressed Air Supply = 4CFM max.
1. Take Z
0
gm ( about 200 gm ) of dry silica sand.
2. To it add W
0
gm of water (75 gm of water)
3. Therefore initial moisture content c
0
(%) is

5 . 37 100
200
75
100
0
0
0

Z
W
c
4. Start the blower and adjust the air flow rate at the desired level.
5. Start the heater and adjust the variac to obtain the desired temperature (i.e 80 to100C). Allow
the air to pass through the bypass line till desired air temperature is reached.
6. Load the conical portion of the drier with the wet material from the top of the column. Close the
lid.
7. Allow the hot air at prefixed flow rate and temperature to pass through the drier. The flow rate
should be sufficient to fluidize the material & record air inlet temperature.
8. At regular intervals of time, take out about 5 gm of wet material and weigh it. Dry it completely
and weigh it again and hence record the % moisture present (c)
9. Continue the experiment till you dont observe appreciable change in the moisture content of the
sample (c
). Stop the supply to the heater first and then switch off the compressor.
10. Repeat steps 1 to 9 for different air flow rates and hot air temperatures.
SPECIFICATION:
1. Process Column
Material = Borosilicate Glass
Conical Portion:
Internal Diameter = 77mm
Height = 97mm
Straight Portion:
Internal Diameter = 74mm
Height = 500mm
2. Fluidizing Material = Silica Sand
Size = < 1mm
3. Heating Capacity = 2.0 kW (2 No., 1kW each)
4. Temp. Measurement = with temperature Indicator
119
5. Control Panel comprises of = Digital temp. controller : 0 199.9C
6. Standard make on/off Switch, Mains Indictor etc.
FORMULAE:
% Moisture present is sample c, =
100
solid dry of wt.
water of wt.
Fraction of water removed, =

( )
( )
c c
c c
0
0
Initial dry wt. of solid = Z
0
gm
Initial moisture content = W
0
gm

0
0
0
Z
W
c
gm of moisture/ gm of dry solid
or
(%) 100
0
0
0

Z
W
c
Air inlet temperature = T
a
OBSERVATION TABLE:
Time, t
(minutes)
% Moisture present in sample, c
(wt of water)/ (Dry wt) 100
Fraction of water removed,
c c
c c
0
0
0 c
0
0
5 ---- ----
10 ---- ----
15 ---- ----
20 ---- ----
c
1
: Large time or till c remains constant.
Plot c vs t
Determine c at t &
Estimate
Plot vs t and get the drying curve.
PRECAUTIONS & MAINTINENCE INSTRUCTIONS:
1. Dont switch on the heaters before starting the blower.
2. Water bottles for wet bulb temperature should be filled with water and the bulb cloth should be
dipped in water.
3. After completion of experiment remove the glass column carefully by opening the flange joints.
120
4. Flow should not be higher than the fluidization velocity.
TROUBLESHOOTING:
2. If switch ON the heater but temperature cant rise but panel LED is ON it means heater had
CONCLUSIONS:
==== X ====
121

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JAYPEE UNIVERSITY OF ENGINEERING & TECHNOLOGY, GUNA

Department of Chemical Engineering

Packing = Raschig rings

Conc. of Benzoic Acid in the Toluene at bottom, C

Amount of Benzoic acid extracted by water A

Amount of Benzoic acid recovered by water A

Average amount of Benzoic Acid recovered,

(using the equilibrium data)

Wt. of product collected - W

is plotted, which is called Breakthrough Curve. A curve between W

= Optical density of fluid at exit at time .

MASS TRANSFER OPERATIONS LAB

Crystal yield = Feed Mother Liquor

Conc. of feed solution at 50C = 1.9856 gm MgSO

Crystal Yield = ---------kg

.. {Ref: B.K Dutta, Principle of Mass transfer

MASS TRANSFER OPERATIONS LAB

Superficial air flow rate G =

(Hold up of dispersed phase)/(Effective volume of column, V

Volumetric rate of extraction of Benzoic acid, kmol/m

Overall Volumetric mass transfer coefficient (1/s) is thus defined as:

Conc. of Benzoic Acid in water at the outlet :

Effective Volume of Toluene = V

OBSERVATION AND CALCULATION:

Dispersed phase superficial velocity, V

MASS TRANSFER OPERATIONS LAB

Effective Volume of Toluene = V

= fraction of water removed from the material.

= % moisture based on dry wt.

= final equilibrium moisture content ( at t )

Fraction of water removed, =

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