Mass Transfer Lab Manual

MASS TRANSFER
OPERATION
LABORATORY MANUAL
Department of Chemical Engineering

School of Technology
Pandit Deendayal Energy University
(Formerly PDPU)
Gandhinagar-382007
Instructions
 Carry the following things while attending the lab session:
 Lab Coat
 Lab manual
 Calculator
 Without above 3 things you will not be allowed to enter in the lab and marked absent
for that particular day
 Shoes are mandatory
 After attendance you will directed to move to the allotted group table/Instrument
 Group movement in lab for different experiments will be told to you before lab sess10ns
 Lab report is to be submitted in next lab. You will need to finish it in that week
 Bags, books, edibles, cell phones, laptops, walkman, iPods etc are not allowed inside UG lab.
Those will be confiscated if found.
 Indiscipline of any sort will not be tolerated and will attract punitive measures
DOs and DON'Ts in the Laboratory
 Do thoroughly clean the glassware before and after use

 Do handle the glassware carefully
 Do not handle chemicals with bare hands
 Do not blow out the last drop from the pipette. When the liquid has drained out
completely, touch the tip of the pipette to the inner surface of the vessel
 Do not add water to acids. Do always add acid to water
 Do use large volumes of water, when a person is splashed with acid to prevent serious
burns
 Do weigh the articles in a balance only at room temperature
 Do use different pipette for different reagents
 Do not pipette out acids and other toxic reagents by mouth
 Do read the level of the curve (meniscus), in all volumetric glassware, with the eye at
approximately the same level as the curve of solution.
Mass Transfer Operation
Lab Report
School of Technology
Department of Chemical Engineering
Pandit Deendayal Energy University (Formerly PDPU)
Student Name: ABC
Student Id: XXBCH0XX
Semester: ………
Session: ……….
Certificate
This is to certify that Mr/Ms …………………………………………………………
Roll No ………………… of Fifth Semester, B. Tech., Chemical Engineering Department, SoT, PDEU
has satisfactorily completed their term work for laboratory course on Mass Transfer Operation Lab –
I/II in Jan-July/July-Dec 20… session.
Dr. Manish Kumar Sinha
Lab In-charge - MTO

Certificate
This is to certify that Mr/Ms …………………………………………………………
Roll No ………………… of Fifth Semester, B. Tech., Chemical Engineering Department, SoT,
PDEU has satisfactorily completed their term work for laboratory course on Mass Transfer Operation
Lab – I/II in Jan-July/July-Dec 20… session.
Dr. Manish Kumar Sinha
Lab In-charge - MTO
5
CONTENTS:
Sr. Name of the experiment Page.
no No.
1 Crystallization of Benzoic acid 06
2 Differential Distillation 09
3 Adsorption of acetic acid 11

4 Solid in air diffusion 16
5 Vapour in air diffusion 21
6 Solid Liquid extraction 27
7 Water cooling tower 29
8 CO2 absorption in NaOH solution in Packed, Sieve plate and 34

wetted wall column)
9 Liquid Liquid extraction (effect of time) 38

10 Liquid Liquid extraction (phase ratio) 42
11 Liquid Liquid extraction (number of stages), 44
12 Liquid-Liquid extraction in a packed bed 48
13 Steam Distilation 53
14 Vapor liquid equilbrium 57
15 Bubble cap distillation column 62
16 Drying of Porous/Nonporous material 71
6
Experiment- 01
CRYSTALLIZATION
OBJECTIVE:
To determine the yield of benzoic acid crystal
INTODUCTION:
Crystallization is an important operation in processing as a method of both purification and of providing
crystalline material in a desired size range. In a crystal the constituent molecules, ions or atoms are
arranged in a regular manner with the result that the crystal shape is independent of size and if a crystal
grows each of the faces develops in a regular manner.
Crystallization is the process where a solid separates from the solution. A saturated solution 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. Crystallization is the formation of solid particles within a
homogenous phase. Its wide use has a twofold basis a crystal formed from an impure solution is itself
pure and crystallization affords a practical method of obtaining pure chemical substance in a satisfactory
condition for packing and storing. This operation involves both heat and mass transfer.
The simplest and cheapest type of crystallization consist of an open tank/vessel which can be used either
as an evaporative or as a cooling crystalline. In batch crystallization process the solvent evaporated until
the concentration has reached the required value, and cooling is then effected by transfer of sensible
heat to the surroundings and evaporation at the free surface. The solution cools slowly and large crystals
are therefore obtained through generally they are uneven because the nucleation is not controlled in
anyway.
The yield of crystals produced by a given cooling may be estimated from the concentration of the initial
solution and solubility at the final temperature allowing for any evaporation by making solvent and
solute balances as follows.
For the solvent, usually water the initial solvent present is equal to the sum of the final solvent in the
mother liquor the water of crystallization within the crystals and any water evaporated,
𝑅−1
𝑊1 = 𝑊2 + 𝑦 + 𝑊1 𝐸
𝑅
Where W1 and W2 are the initial and final masses of solvent in the liquor, y is the yield of crystals, R
is the ration (molecular mass of hydrate/ molecular mass of anhydrous salt) and E is the ratio (mass of
solvent Evaporated/mass of solvent in the initial solution). For The solute
𝑦
𝑊1 𝑐2 = 𝑊2 𝑐2 +
𝑅
Where C1 and C2 are the initial and final concentration of the solution expressed as (mass of anhydrous
salt/mass of solvent) substituting for W2 we get yield as
𝑐1 − 𝑐2 (1 − 𝐸)
𝑦 = 𝑅𝑊1
1 − 𝑐2 (𝑅 − 1)
Batch crystallization is characterized by the fact the system is always in the unsteady state. The initial
super saturation at which crystallization starts will drop quickly 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 the 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
7
producing a fine mass of fine crystals. By using controlled seeding the solution will not become labile
there by aiding crystal growth.
Utilities Required:
Distilled Water, Benzoic Acid, Thermometer, Glass Rod, Hot Plate.
EXPERIMENTAL PROCEDURE:
1. Figure shows the experimental setup for a batch crystallizer. Hot plate is used to heat the
solution to the desired temperature. Glass rod for stirring, thermometer for temperature
measurement.
2. Take a known quantity of distilled water (200 ml) in a flask and heat it to 60 ° C on a hot plate
3. Keep on adding the weighted amount of benzoic acid with simultaneous stirring by a glass rod,
until benzoic acid stop dissolving. Note down the total amount of benzoic acid that was
dissolved.
4. Now remove the flask from the hot plate and allow it to cool.
5. Put 0.2 gm benzoic acid in the crystallizer when the temp reduces by 5°C, for seeding.
6. Keep the system for about two hours and continuously record the temperature of the system
after each 10 min.
7. Note down the final temperature of solution at each interval
8. After formulation of crystal filter the solution
9. Measure the amount of mother liquor obtained and titrate the solution with 0.1 N NaOH
10. Collect all the crystal from the mesh on a filter paper wash it and put it in oven for drying.
11. Weigh the dried crystal obtained
OBSERVATION TABLE:
Obs.
No
1 Amount of benzoic acid dissolve in feed = …………………… gm
2 Volume of feed = ………………………………….ml
3 Burette reading for 10 ml feed soln. titration against 0.1 N
NaOH=………………………ml
4 Volume of filtrate =………………….. ml
5 Burette reading for 10 ml filtrate titration against 0.1 N NaOH=………………………ml
CALCULATION:
Normality of feed N1 = N2 V2 / V1
Amount of benzoic acid in feed = N1 * Eq. Wt * volume of feed = ……………… gm
Normality of benzoic acid in filtrate N1 = N2 V2 / V1
Amount of benzoic acid in filtrate = N1 * Eq. Wt * volume of filtrate (lit) = ……………… gm
Weight of crystals = amt. of B.Acid in filtrate
8
𝑐𝑟𝑦𝑠𝑡𝑎𝑙𝑠 𝑜𝑏𝑡𝑎𝑖𝑛𝑒𝑑
% efficiency of crystallization = 100%
𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑏𝑒𝑛𝑧𝑜𝑖𝑐 𝑎𝑐𝑖𝑑 𝑖𝑛 𝑓𝑒𝑒𝑑
= ……………….%
RESULT:
%Efficiency of crystallization = ………………………………..
RESULT & CONCLUSION:
9
Experiment- 02
DIFFERENTIAL DISTILLATION
AIM:
To preform differential equation experiment and verify the Rayleigh equation
THEORY
Differential equation is also known as the batch distillation or simple distillation. The mixture
is charged to a still or rebo:1,:r and heat is supplied through a coil or through the wall of the
vessel to bring the liquid at boiling point and vaporize the part of the batch. In the simplest
method of operation the vapor is taken directly from the still to a condenser. The vapor leaving
the still at any time is in equilibrium with liquid in the still but since the vapour phase is richer
in more volatile component the composition of vapor and liquid phase is not constant.
Over a small time the change in the amount of liquid in the still is dL and the amount of vapour
withdrawn is dD the following differential mass balance equation may be written
Total material balance: -dL = dD
Component A balance: -d(Lx) = Y*dD
From these two equation on simplification we can get
𝑑𝐿 𝑑𝑥
= ∗
𝐿 𝑦 −𝑥
If distillation starts with F moles of concentration XF and continues till the amount of amount
of liquid reduces to W moles (composition = xw), the above equation can be integrate to give
𝑊 𝑋𝑤
𝑑𝐿 𝑑𝑥
∫ = ∫
𝐹 𝐿 𝑋𝐹 𝑦∗−𝑥
The relation starts between V and X can be found out by introducing relative volatility and
solving above equation we will get
𝐹 1 𝑋𝐹 (1 − 𝑋𝑊 ) (1 − 𝑋𝑊 )
𝐼𝑛 = 𝐼𝑛 + 𝐼𝑛
𝑊 (𝑎 − 1) 𝑋𝑊 (1 − 𝑋𝐹 ) (1 − 𝑋𝐹 )
PROCEDURE
1. Clean the apparatus and connect all the connect water supply to the condenser
2. Take 100 ml of methanol and 100 ml of water in the still
3. Start the water circulation through the condenser
10
4. Start the heating of solution Heat the solution in the still at a constant temperature at
about 80°C .
5. Collect the distillate and residue in measuring cylinder and determine the concentration
of methanol by using refractometer
6. Note down the total volume of distillate and remaining volume of residue
7. Repeat the experiment at different pre-specified time interval
APPARATUS
Experimental Setup
OBSERVATION TABLE
Feed T1 T2 T3 T4 T5
Volume
Feed
Composition
Residue
volume
Residue
composition
Distilled
volume
Distilled
composition
11
CALIBRATION DATA
S. No. Mole fraction of A RI

1 0
2 0.1
3 0.2
4 0.3
5 0.4
6 0.5
7 0.6
8 0.7
9 0.8
10 0.9
11 1.0
CALCULATIONS
Put all the values of F, W, XF, Xw, in equation number 5 and verify the Rayleigh equation
Also plot the graph of (1/(Y* - x)) vs x and determine area under the curve in the range of Xf
Xv, and verify equation number 4 Result and discussion:
CALCULATIONS TABLE
S No. (1/(Y* - x)) x
CONCLUSION:
12
Experiment- 03
ADSORPTION
OBJECTIVE
 The aim of this experiment is to study the adsorption of acetic acid by solid adsorbent
activated carbon and then test the validity of certain adsorption isotherm.
PRINCIPLE AND THEORY
Adsorption is a process that uses special solids to remove substances from either gaseous or
liquid mixtures. It is an industrially important process occurs with the attachment of the gas
particles onto a solid surface. The special solids that gas or liquid particles attached are called
adsorbent. The substances adsorbed are called adsorbate. Adsorption is a phenomenon occurs
at the surface; the molecules are taken up by the surface. It should not be confused with
absorption. Adsorption and absorption are two different processes: the molecules are taken
up by the volume in absorption, not by surface i.e. the solute is dissolved in the bulk material
in absorption. Adsorption can be classified into two different groups depending on the type
interaction between the adsorbed molecule and the solid surface.
 Physisorption ;-Physisorption is caused mainly by intermolecular forces(Van der

Waals) and electrostatic forces between adsorbate molecule and the atoms which
compose adsorbent surface. It will occur when the intermolecular attractive forces
between and adsorbent and adsorbate are greater than those existing between
molecules of the adsorbate itself.
 Chemisorption;- Chemisorption is the result of chemical interaction between
adsorbate and adsorbent. The adsorbate sticks to the solid by the formation of a
chemical with the surface. This interaction is much stronger than
physisorption. Unlike in physisorption only monolayer adsorption is observed.
Activated carbon is basically amorphous carbon based material exhibiting a high degree of
porosity and interparticulate surface area. large surface area of activated carbon provides
excellent adsorbent characteristics. The surface area per gram of material can range 500 to
2000 m2. Because of its good adsorption properties they are useful in many industrial
processes. Filtration, purification, deodorization, decolorization and separations are the
examples of processes.
Adsorption Equilibrium ;
13
A large majority of adsorption operate through equilibrium adsorption of mixture. The amount
of gas or liquid adsorbed, na by mass, per gram of solid, ms, depends on the specific surface
area of the solid, the equilibrium solute concentration in the solution on, Ceq (pressure for gas
phase adsorption), the temperature, and the nature of the molecules involved. For the given
system at constant temperature it is possible to write the adsorption isotherm equation as
follows
qeq= na / ms = f (Ceq) (1)
where qeq is the amount of adsorbate per unit mass of adsorbent.
The most common way of getting information about a given system is to take experimental
measurements, at constant temperature, of the amount of adsorbate on the surface as a
function of concentration(or pressure) and then draw a plot of qeq (the amount of adsorbate per
unit mass of adsorbent) versus Ceq(the equilibrium solute concentration in adsorption from
solution). Such a graph is called an adsorption isotherm.
The Freundlich isotherm
It applies over a limited range of concentrations and is somewhat better for liquid –solid
systems. It has the form of
qeq= na / ms K. (Ceq)a (2)
where, na Amount of the adsorbate(grams) & ms = Amount of the adsorbent
In Eqn (2) K and a are constants.
The Langmuir Isotherm
The theory of Langmuir is restricted to cases where only one layer of molecule can be adsorbed
on the surface. As mentioned before, in the case of chemisorption monolayer adsorption is
usually observed. The monolayer adsorption is distinguished by the fact that amount adsorbed
reaches a maximum value at moderate concentrations(corresponding a complete coverage of
the surface of the adsorbent by a layer of adsorbed molecules which is one molecule thick
only), and remains constant with further increase in concentration. The equation of Langmuir
as derived for the chemisorption of gases is:
14
𝜃 = K.( Ceq) /(1+K . Ceq) (3)
where,
𝜃 : Fraction of the solid surface covered by the adsorbed molecules
K: Adsorption equilibrium constant
Ceq: Equilibrium concentration
Langmuir isotherm equation can be written for the gas adsorption by replacing C by P, also
note that
∅ = qeq / qmeq (4)
where qmeq is the amount of adsorbate per unit mass of adsorbent required to form a
monolayer.
Hence Eqn 3 takes the form of
qeq / qmeq = K.( Ceq) /(1+K . Ceq) (5)
Ceq / q = Ceq / qmeq + 1/(K . qmeq ) (6)
Chemical :- Activated carbon, Acetic acid, Sodium Hydroxide, Phenolphthalein,

Hydrochloric acid, Potassium Hydrogen phthalate.
EXPERIMENTAL PROCEDURE
In this experiment it is important to measure the acetic acid concentration accurately. To this
end the NaOH solution must be titrated with standard 0.1M HCL solution and then titrated
with the acetic acid solution.
1. Weight out 0.3 g of activated into each of 5 clean stoppered 125ml conical flasks
2. Add 40 ml of 0.20M acetic acid (Stock Solution) to the first flask and shake. Then add
40mL to each of the other flasks at concentration of 0.15M, 0.10M and 0.05M
3. Shake each loosely stoppered flask periodically over 30 minutes noting the room
temperature. Then filter each solution through a filter paper ( to completely remove
charcoal particles). It is important that the equilibrium acetic acid concentration be
accurately determined
15
4. Pipet two 10mL potion of each filtrate add a few drops of phenolphthalein indicator
and titrate with 0.1 M/N NaOH. Record the volume of NaOH used.
Data Analysis
Calculate the no. of acetic acid molecules adsorbed per gram of charcoal (qmeq) and the
corresponding equilibrium acid concentration (Ceq). plot qmeq against Ceq and Ceq / qmeq
against Ceq . Determine the surface area per gram of charcoal assuming that one adsorbed acetic
acid molecule occupies an area of 21x 10-10 m2.
RESULTS AND CONCLUSION
Estimate the value of the equilibrium constant K with the correct units.
PRECAUTION AND MAINTENANCE

 Always use gloves for handling the acid/base.
 Proper cleaning should be necessary for the setup and glassware.
16
Experiment- 04
SOLID IN AIR DIFFUSION

OBJECTIVE:
 To calculate the mass transfer coefficient for vaporization of naphthalene in air using a
packed bed of spherical particles of naphthalene.
 To plot (Sh / Sc)1/3 vs Re on a log-log graph and determine the functional relationship.
INTRODUCTION:
Diffusivity at solids are lower values than, liquids and gases. Diffusion plays a major role in
catalysts and is important to chemical engineers. Diffusion at atoms within the solids is of more
importance.
THEORY:
For component A (naphthalene) diffusing through non-diffusing B (air) at ambient temperature,

with diffusivity coefficient DAB in packed bed of sphere particle
Then mass transfer coefficient can be calculated by following correlation:
Where Re is Reynolds number, Dp is diameter of the particle (naphthalene), V is velocity of

air, 𝜌 is the density of the air and 𝜇 is viscosity of the air.
𝜇
𝑠𝑐 = … … … … … … … … … … … … … … … … … … . . (𝐵)
𝜌 𝐷𝐴𝐵
Where Sc is the Schmidt number and DAB diffusivity coefficient
𝑆ℎ = 1.17𝑅𝑒 0.585 𝑆𝑐1/3 … … … … … … … … … … … … … … … … … … … … … … . (𝐶)

Where Sh is Sherwood number
𝑆ℎ ∗ 𝐷𝐴𝐵
𝐾𝑐 = … … … … … … … … … … … … … … … … … … … … (𝐷)
𝐷𝑝
Kc is mass transfer coefficient
17
DESCRIPTION:
The equipment is fitted with a vertical glass column with a mesh near the base of column to hold
the spherical balls. Spherical balls of known diameter are filled in the column to make a packed
bed. Air is allowed to pass through the silica gel member. From the bottom of the column, dry air
is allowed to enter in the packed bed. Rotameter is provided to measure the flow rate of air.
1
XA=0
Q {LPM}
Starting procedure:
1. Pack the glass tube with known number and known diameter of naphthalene balls up to a
height of about 15 cm.
2. Record the average diameter of the naphthalene ball.
3. Connect the air line from the compressor to the valve V2 at the base of the column.
4. Note the ambient temperature.
5. Open the valve V1 and set the flow rate of air.
6. Allow the air to flow through the packed bed for a fixed time (say 60 min).
7. Record the flow rate of air.
8. Repeat the experiment for different flow rate of air.
Closing procedure:
1. When experiment is over remove the balls from set-up.
2. Remove the connection of compressed air supply.
18
CALCULATION
4𝑊
𝑁𝐴 =
𝑀𝐴 𝜋𝐷2 𝑡 ∗ 60
𝑀𝑎𝑖𝑟 𝑊 ∗ 1000
𝑋=( )( )
𝑀𝐴 𝑄𝑡𝜌𝑎𝑖𝑟
𝑃𝐴 = 𝑋𝑃
ln{(𝑃𝐴𝑆 )1/(𝑃𝐴𝑆 − 𝑋𝑃)2}
𝐾𝑃 = 𝑁𝐴 [ ]
(𝑃𝐴𝑆 )1 − (𝑃𝐴𝑆 − 𝑋𝑃)2
RESULTS:
(Method 1)
Mass transfer coefficient 𝐾𝑃 at different flow rate are tabulated below and graph shows the
nature of 𝐾𝑃 at different flow rate
S. Flow rate (LPM) Molar flux Molar Partial Mass transfer

NO 𝑁𝐴 fraction of pressure of coefficient
naphthalene naphthalene 𝐾𝑃 (mole/m2.sec)
“X” 𝑃𝐴 (𝑝𝑎𝑠)
Alternative calculation for mass transfer coefficient

𝜋
𝐴= × (𝐷𝑐)2 (𝑚2 )
4
𝑄 𝑚
𝑉= ( )
𝐴𝐶 ∗ 1000 ∗ 60 𝑠
𝐷𝑃 𝑉𝜌
𝑅𝑒 =
𝜇
𝜇
𝑆𝐶 =
𝜌𝐷𝐴𝐵
𝑆ℎ = 1.17𝑅𝑒 0.585 𝑆𝑐1/3
19
𝑆ℎ𝑋𝐷𝐴𝐵
𝐾𝐶 =
𝐷𝑃
(Method 2)
SI NO Flow rate 𝑅𝑒 Sc Sh 𝐾𝐶
 Compare the value of Kc and Kp obtained by two different methods.

 Draw the graph between (Sh/Sc)1/3 vs Re on log – log graph
BLOCK DIAGRAM:
20
RESULT & CONCLUSION:
PRECAUTION & MAINTENANCE INSTRUCTIONS:

 Air pressure should be constant during the experiment.
 Silica gel should be dry.
 Don’t exceed the pressure above 1kg/cm2.
21
Experiment- 05
VAPOR IN AIR DIFFUSION

OBJECTIVE:
 To determine the diffusion coefficient (DAB ) of acetone (A) in air (B).
 To study the effect of temperature on the diffusion coefficient.
THEORY
Diffusion is concerned with the movement of individual molecules through a substance by
virtue of their thermal energy. In the diffusion process, the molecules of interest flow from
region of high concentration to low concentration. Mathematically diffusion is governed by the
equation 1.1
NA=XAN+JA=XA (NA+NB) + JA………………………….(1.1)
Where NA = total molar flux of A, XA= mole fraction of A in the mixture of A and B, N is the
total flux of A and B with respect to the stationary observer, JA= flux of A due to molecular
diffusion
The molecular diffusion “JA” is given by the fick’s law as in equation (1.2)
𝑑𝐶𝐴
JA = -DAB (𝐶𝐴1 > 𝐶𝐴2 )in the increasing direction of z) …………………(1.2)
𝑑𝑧
DAB is diffusivity coefficient of A diffusing in B. it is defined as the amount of mole of A

diffused per unit time when concentration gradient of A along the decreasing concentration
path is unity. Its SI unit is m2/s.
In case of steady state diffusion of A through stagnant B, NB = 0 equation 1.2 transforms to

𝑑𝐶𝐴
NA = XA (NA) -DAB … … … … … … … … … … … … (1.3)
𝑑𝑧
For ideal gas law
𝑃 𝑑𝑃𝐴
NA dz= -DAB 𝑅𝑇 ………………………………… (1.4)
𝑑𝑧
22
Where P is total pressure PA is the partial pressure of A in mixture of A and B. on integrating
equation 1.4 within limit Z = (0,Z) and PA=(PA1,PA2) respectively we get
𝑝 𝑃−𝑃
NAZ=DAB𝑅𝑇 𝑙𝑛(𝑃−𝑃𝐴2 )…………………………….. (1.5)
𝐴1
Equation 1.5 is derived by taking an assumption of pseudo steady state in which N A is not
changing with time. Equation 1.5 when applied to Stephen tube experiment can be used to find
out mole of liquid diffusing at a particular instant and level of liquid in the tube shown in fog
1.1 figure shows the process of diffusion of acetone in air. In this case air is stagnant and it will
not diffuse in liquid. At the upper part of tube gentle air is flowing so the liquid vapors are not
accumulated. We can assume that air quality is large enough so that the composition of vapor
is negligible at top position.
At the interface of air and liquid we can assume vapor pressure of liquid “PAO” equals the
partial pressure of acetone at that temperature.
Gentle flow of air

PA =0
Z1
t=0
Z2
t=∆𝑡
PA=PA0
Figure 1.1 Stephen tube containing liquid diffusing under gentle flow air
After sometime “"∆𝑡" liquid level decrease from Z1 to Z2 due to diffusion. The unsteady state
situation can also be assumed to be pseudo steady state assumption as acetone level decrease
very slowly.
Putting the value of PA1 and PA2 in equation 1.5 gives equation 1.6
𝑝 𝑃
NAZ=DAB𝑅𝑇 𝑙𝑛(𝑃−𝑃 )……………………………………….(1.6)
𝐴0
Amount (mole) of liquid diffuses in time interval “"∆𝑡" is given by
23
Na * A * ∆𝑡…………………………………………………(1.7)
This amount is responsible for the decrease in the level of acetone thus
𝜌
Na * A * ∆𝑡 = (Z1-Z2)A 𝑀𝐴 ……………………………………(1.8)
𝐴
Putting the value of NA this equation can be written as

𝑝 𝑃 𝜌𝐴 𝑑𝑧
DAB𝑅𝑇 𝑙𝑛 (𝑃−𝑃 ) = ( 𝑑𝑡 ) …………………………………(1.9)
𝐴0 𝑀𝐴
On integrating we get
1 𝜌 𝑅𝑇 𝑃 𝑍12 −𝑍22
DAB = ∆𝑡 (𝑀𝐴 ) ( 𝑃 ) ln (𝑃−𝑃 ) ( )………………………………… (1.10)
𝐴 𝐴0 2
Usually the absolute value of Z is not available or not measured during the experiment. In
spite of this value of (Z1-Z2) can be found out experimentally hence equation 1.10 can be
written as
∆𝑡 𝜌𝐴 𝑅𝑇 𝑃 𝜌𝐴 𝑅𝑇 𝑃
= ln( )(𝑍1 − 𝑍2 ) + ln( )𝑍2…………….(1.11)
𝑍1 −𝑍2 2𝐷𝐴𝐵𝑀𝐴 𝑃 𝑃−𝑃𝐴0 𝐷𝐴𝐵𝑀𝐴 𝑃 𝑃−𝑃𝐴0
∆𝑡
Plotting the value 𝑍 VS Z1-Z2 should yield a straight line with slope
1 −𝑍2
𝜌 𝑅𝑇 𝑃
S= 2𝐷 𝐴 ln(𝑃−𝑃 )……………………………………………… (1.12)
𝐴𝐵𝑀𝐴 𝑃 𝐴0
Thus from equation 1.12

𝜌 𝑅𝑇 𝑃 1
DAB = 2𝐷 𝐴 ln (𝑃−𝑃 ) 𝑆………………………………………… (1.13)
𝐴𝐵𝑀𝐴 𝑃 𝐴0
EXPERIMENTAL SET UP
The equipment consist of a T tube made of glass, placed in a water bath. Water bath is provided
with heater. Temperature of the bath is controlled by the digital temperature controller. Stirrer
is given to maintain the constant temperature in bath. Air pump is provided to supply the sir,
passed through the tube. Change in the liquid level is observed by the travelling microscope
with sliding venire scale.
1. Before switching on the power clean the apparatus, T tube and fill the water bath with
water 3/4th of its capacity.
2. Set the water bath temperature (between 35ºC to 50ºC)
3. Switch ON the heater and stirrer
4. Wait till the bath attains the set temperature. Note the steady temperature of the bath.
5. Fill the T- tube with acetone solution up to 2cm. of the capillary leg.
6. Note down the initial height of liquid in the capillary as (Z1)
7. Make the connection with air pump and allow a gentle current of air to flow over the
capillary.
8. Record the height of liquid in the capillary after every 20 min as (Z2)
24
9. Repeat the experiment for 5 diff. water bath temperature (between 35ºC to 50ºC)
10. Plot diffusion co efficient against absolute temperature on a log-log graph and
determine the slope.
11. When exp. Is over stop the air supply, switch OFF heater and stirrer, switch OFF the
main power supply and clean the tube and drain the water bath.
OBSERVATION AND CALCULATION

1.6 Data Value
Total pressure (P)
Real gas constant (R)
Molecular wt. of liquid (MA)
Density of liquid ((𝜌𝐴) at temperature T1
Partial press. Of liquid at top of tube (PA1) at temperature T1
OBSERVATIONS
Observation table:
S NO Temperature Initial time Final time Initial Final height
(℃) height (cm) (cm)
CALCULATION
To find the diffusivity of acetone in air

∆𝑡
Plot the value 𝑍 VS Z1-Z2
1 −𝑍2
From the slope of the straight line (S) diffusivity coefficient can be calculated as
𝜌 𝑅𝑇 𝑃 1
DAB = 2𝐷 𝐴 ln (𝑃−𝑃 )
𝐴𝐵𝑀𝐴 𝑃 𝐴0 𝑆
Similarly repeating the calculation at different temperature we get different valves for
diffusion coefficient. Draw log –log between temperature and diffusivity
DAB = cTn
25
Find the value of n to relate temperature dependence of diffusivity
RESULT AND DISCUSSIONS
Diffusivity of acetone found at temperature is shown in following table and graph
Sr. No Temperture ℃ Diffusivity (m2/s)

1
2

 Temperature should be constant during the experiment.
Don’t run heater without water.
BLOCK DIAGRAM
26
Experiment- 06
SOLID LIQUID EXTRACTION

OBJECTIVE:
To study solid liquid extraction in batch process and hence find out the effect of solvent
temperature on the percentage recovery of oil from oil seeds.
THEORY
Leaching is method of extraction a desired chemical that is dispersed or dissolved in a solid.
The solid is ground up into small pieces and wasted with a solvent in which the desired
chemical is soluble. Sometimes the solid and solvent from slurry that can be conveyed easily.
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 of otherwise purified.
The laboratory experiment uses simple equipment to explore a leaching operation that is
familiar to all of us the extraction of oil from seeds using hexane as the leaching solvent.
Some of the parameters affecting the leaching efficiency are
 Extraction time
 Extraction temperature
 Size of the solid particles
 Type and amount of solvent used
Utilites
Hot plate, Beaker, Thermometer, Hexane, Oilseed, Oven
1. Leaching process was studied for the extraction of oil from the cotton/castor seed oil
using hexane or methanol as the solvent.
2. 500ml of Hexane is taken in a beaker and raised to predetermined temperature.
3. Note down the temperature
4. Add known weight of cotton/Caster seed paste in a beaker.
5. Mix the sample for 30 min.
6. Filter the mixture and keep the solid material for drying in an oven.
7. After drying sample was weighted.
8. Repeat the experiment for different temperature.
27
OBSERVATION AND CALCULATION
Observation table
SI. NO T (º C) Initial Initial wt of Final wt of Final volume
Volume of oilseed (g) oilseed (g) of solvent
Solvent (ml) (ml)
CALCULATION
intial weight − final weight
% extraction = × 100
intial weight
CALCULATION TABLE
SI. No T (º C) % extraction
RESULT AND DISCUSSIONS

 Always use the fresh oilseed.
 Hexane/Methanol should be oil free or not used.
 Proper cleaning should be necessary for the set up.
28
Experiment- 07
WATER COOLING TOWER
OBJECTIVE:
 To study mass transfer operation in water cooling tower for different flow and thermodynamic
conditions.
 To calculate the tower characteristic of water cooling tower for various liquid and air flowrates.
INTRODUCTION:
Water from condensers and heat exchangers is usually by an air stream in spray ponds or in cooling
towers using natural draft or forced draft by flow of the 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. Markel’s theory is used which is based on enthalpy potential difference as the driving force.
For mass transfer operation:
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
from Markel’s equation can be written as:
𝑇5
𝐾𝑎 𝑉 𝑑𝑇
= ∫
𝐿 𝑇0 ℎ𝑊 − ℎ𝑎
Tower characteristic can be evaluated numerically by:

𝑇5
𝐾𝑎 𝑉 𝑑𝑇 (𝑇5 − 𝑇6 ) 1 1 1 1
= ∫ = ∗( + + + )
𝐿 ℎ𝑊 − ℎ𝑎 4 ∆ℎ1 ∆ℎ2 ∆ℎ3 ∆ℎ4
𝑇6
1 1 1 1 1
if = ( ∆ℎ + ∆ℎ + ∆ℎ + ∆ℎ )
∆ℎ 1 2 3 4
Then the above equation becomes:

𝐾𝑎 𝑉 (𝑇5 − 𝑇6 ) 1
= ∗
𝐿 4 𝛥ℎ
ℎ𝑤1 = 𝑇6 + 0.1(𝑇5 − 𝑇6 )
ℎ𝑤2 = 𝑇6 + 0.4(𝑇5 − 𝑇6 )
ℎ𝑤3 = 𝑇5 + 0.4(𝑇5 − 𝑇6 )
ℎ𝑤4 = 𝑇5 + 0.1(𝑇5 − 𝑇6 )
ℎ𝑎1 = ℎ1 + 0.1(𝐿⁄𝐺 )(𝑇5 − 𝑇6 )
29
ℎ𝑎2 = ℎ1 + 0.4(𝐿⁄𝐺 )(𝑇5 − 𝑇6 )
ℎ𝑎3 = ℎ2 − 0.4(𝐿⁄𝐺 )(𝑇5 − 𝑇6 )
ℎ𝑎4 = ℎ2 − 0.1(𝐿⁄𝐺 )(𝑇5 − 𝑇6 )
𝐾𝑎 𝑉
Where is tower characteristics also called mass transfer coefficient group, Δh is summation
𝐿
of reciprocal of enthalpy difference. Hw1 – Hw2 are enthalpy of water, ha1-ha4 are enthalpy
of air. L/G is liquid to air flow ratio. H1-h2 are enthalpy of air at wet bulb temperature.
The carrying of liquid the 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.
DESCRIPTION:
The set-up consists of tower which is forced draft counter current type. Fan is provided at the
bottom of the tower. There is an orifice meter mounted with its taps connected to a manometer
to measure the flow rate of air. Butterfly valve is given to control the air flow rate. Nozzles are
provided for distribution of water on the packing. Rotameter is given to control the water flow
rate. A water tank at the bottom fitted with level gauge is provided. Magnetic pump is provided
for circulation of hot water. Temperature sensors are provided to measure the dry bulb and wet
bulb air temperatures. The cooling tower is packed with aluminium expanded wire mesh.
Starting procedure:
1. Close all the valves V1 – V5
2. Ensure that switches given on the panel are at OFF position
3. Open the valve V1 and fill the water
4. Connect electric supply to the set up
5. Set the desired water temperature in the DTC by operating the increment or decrement
and set button of DTC
6. Open by pass valve V3 and switch ON the pump
7. Switch ON the heater and wait till desired temperature achieves
8. Switch ON the blower
9. Allow hot water to flow through cooling tower and adjust the flow rate by rotameter
and control valve V2
10. Allow air to flow through cooling tower and adjust the flow rate by control valve V4
provided in pipe line
11. At steady state(constant water temperature) record the temperatures
12. Record the flow rate of water and manometer reading
13. Repeat the experiment for different air and water flow rates
Closing Procedure:
1. When experiment is oven switch OFF the heater
2. Switch OFF the pump and blower
3. Switch OFF main power supply
4. Drain the water tank by open the valve V5
30
OBSERVATION AND CALCULATION:
1. Data
Cross sectional area a 0.0225 m2
Diameter of orifice do 0.026 m
Diameter of pipe dp 0.052 m
Coefficient of discharge Cd 0.64
Density of air ρa 1.21 kg/m3
Observation table:
S.No T1 (°C) T2 (°C) T3 (°C) T4 (°C) T5 (°C) T6 (°C) R1(cm) R2 (cm) QW
(LPH)
Calculation:
𝑅1 − 𝑅2 𝜌𝑤
𝛥𝐻 = ( − 1) (𝑚)
100 𝜌𝑎
𝜋 2 2
𝑎𝑜 = 𝑑 (𝑚 )
4 𝑜
𝜋
𝑎𝑝 = 𝑑𝑝2 (𝑚2 )
4
𝑎𝑝 𝑎𝑜 𝑚3
𝑄𝑎 = 𝐶𝑑 √2𝑔∆𝐻 ( )
√𝑎𝑝2 − 𝑎𝑜2 sec
𝑘𝑔
𝑀𝑎 = 𝑄𝑎 𝜌𝑎 ( )
sec
𝑄𝑊 𝜌𝑊 𝑘𝑔
𝑀𝑊 = ( )
1000 ∗ 3600 sec
𝑀𝑎 𝑘𝑔
𝐺= ( )
𝑎 (𝑠𝑒𝑐 ∗ 𝑚2)
𝑀𝑤
𝐿= (𝑘𝑔/ sec 𝑚2)
𝑎
𝐿
𝑅=
𝐺
𝑇𝑤1 = 𝑇6 + 0.1(𝑇5 − 𝑇6 )(°𝐶)
𝑇𝑤2 = 𝑇6 + 0.4(𝑇5 − 𝑇6 ) (°𝐶)
𝑇𝑤3 = 𝑇5 + 0.4(𝑇5 − 𝑇6 ) (°𝐶)
31
𝑇𝑤4 = 𝑇5 + 0.1(𝑇5 − 𝑇6 )(°𝐶)
To calculate the property of water (hw1) at temperature Tw1, (hw2) at temperature Tw2, (hw3)
at temperature Tw3,(hw4) at temperature Tw4.
hW1=…………………... (KJ/kg dry air)
To calculate the property of air (h1) at temperature T2
h1 = ……………………. (KJ/kg dry air)
ℎ1 = ℎ1 + 𝑅(𝑇5 − 𝑇6 )(KJ/kg dry air)
ℎ𝑎1 = ℎ1 + 0.1 ∗ 𝑅(𝑇5 − 𝑇6 )(KJ/kg dry air)
ℎ𝑎2 = ℎ1 + 0.4 ∗ 𝑅(𝑇5 − 𝑇6 )(KJ/kg dry air)
ℎ𝑎2 = ℎ2 − 0.4 ∗ 𝑅(𝑇5 − 𝑇6 )(KJ/kg dry air)
ℎ𝑎4 = ℎ2 − 0.1 ∗ 𝑅(𝑇5 − 𝑇6 )(KJ/kg dry air)
∆ℎ1 = ℎ𝑤1 − ℎ𝑎1 (KJ/kg dry air)
1 1 1 1 1
=( + + + )
∆ℎ ∆ℎ1 ∆ℎ2 ∆ℎ3 ∆ℎ4
(𝑇5 − 𝑇6 )
𝑇𝐶 = ( ∗ ∆ℎ)
4
To plot the graph of TC Vs R

 To plot the graph of TC Vs R

 Always use distilled water.
Make sure the water level in tank before starting the experiment. Never run heater without
water.
32
Experimental setup Diagram
33
Experiment- 08
CO2 ABSORPTION IN NaOH SOLUTION
OBJECTIVE:
 To study the absorption of carbon dioxide by aqueous sodium hydroxide solution in a
sieve plate, packed bed and wetted wall column.
 To calculate the overall mass transfer coefficient (KGa)
 To calculate the number of transfer units (NTU)
 To calculate the height if transfer units (HTU)
THEORY
In the absorption the gas mixture is contacted with the liquid for the preferential dissolution of
one or more component of the gas in liquid. Such operation requires transfer of mass from gas
stream to the liquid. In many industrial application, the absorption process is accompanied by
chemical reaction usually; reaction in the liquid of the absorbed component with a reagent in
the absorbing liquid takes place. The reagent and the product of the reaction may be soluble
e.g. absorption of CO2 into an aqueous solution of ethanol amines or other alkali solution.
Reaction of the absorbed solute provide higher absorption rates due to:
 Destruction of the absorbed solute as it forms a compound reduce the equilibrium
partial pressure of the solute that in turns increases the concentration difference
between the bulk phase and the interface.
 Increase the liquid mass transfer coefficient
Absorption of CO2 can be performed by using different absorption column viz sieve plate,
packed bed and wetted wall column. Extent of absorption in these column depends on the
effective contact between the gas and liquid solution.
Tray towers are vertical cylinder in which the liquid and gas are concentrated in stepwise
fashion on trays or plates. The liquid enters at the top and flows downward by gravity. On the
tray, it flows across each tray and through a downspout to the tray below. The gas passes
upward through opening of the one sort or another in the tray.
Packed bed columns are vertical columns which have been filled with packing of device of
large surface. The liquid is distributed over, and trickles own through, the packed bed
exposing a large surface to contact the gas.
A thin film of liquid running down the inside of vertical pipe, with gas flowing either
concurrent or counter currently, constitutes a wetted wall tower. Such device have been used
for theoretical studies of mass transfer, because of the interfacial surface between the phases
is readily kept under control and is measurable.
34
PROCEDURE
 Start the supply of NaOH to the column and adjust flow rate by opening the valve V1.
 Note down the flow rate of NaOH solution.
 Wait till the overflow, now start the supply of CO2 and compressed air.
 Fix the flow rate of CO2 by opening the valve V3 and compressed air by adjusting the
valve V2.
 Note down the flow rate of CO2 and compressed air.
 Wait for 10 minutes, collect 10ml sample in a conical flask that already contains 25
ml of BaCl2.
 Titrate the sample solution against 0.5 N HCL using phenolphthalein as an indicator.
OBSERVATION
 Atmospheric pressure P = 1 atm
 Diameter of the column dc = 0.048 m (packed bed wetted wall)
 Diameter of the sieve plate column = 0.08 m
 Height of the column h = 0.750 m
Observation table:
QL (LPH) QG (LPM) QA (LPM) V1 (ml) V2 (ml)
Sieve plate
Packed bed
Wetted wall
CALCULATION
𝑁2 𝑉2
𝑁1 =
𝑉1
𝐶0 = 𝑁1
𝜋
𝐴 = 4 𝑑𝑐2
(𝐶𝑖− 𝐶0 )𝑄𝐺
𝑁𝑎𝑏𝑠 = (𝑚𝑜𝑙𝑒/𝑠𝑒𝑐)
2∗60
𝑄 𝐺 ∗ 𝜌𝐺
𝑁𝐺 = (𝑚𝑜𝑙𝑒/𝑠𝑒𝑐)
𝑀𝐺 ∗60
𝑄 𝐴 ∗ 𝜌𝐴
𝑁𝐺 = (𝑚𝑜𝑙𝑒/𝑠𝑒𝑐)
𝑀𝐴 ∗60
𝑁𝐺
𝑌1 = 𝑁𝐺 + 𝑁𝐴
35
BLOCK DIAGRAM

Don’t exceed the pressure above 1kg/cm2
36
Experiment- 09
LIQUID -LIQUID EXTRACTION
(Effect of time)
OBJECTIVE:
To determine the effect of time on extraction efficiency and find out the optimum time for
maximum percentage extraction.
THEORY
Liquid - liquid extraction, sometimes call 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 distributes themselves differently between the two liquid
phase a certain degree of separation will results and this can be enhances by use of multiple
contact or their equivalent in the manner of gas absorption and distillation.
Extraction equipment may be operated batch wise or continuously. A quantity oil feed liquid
may be mixed with a quantity of solvent in an agitated vessel (separating funnel), after which
a layer are settled and separated. The extract is the layer of solvent plus extracted solute, and
the raffinate is the layer from which solute has been removed. The extract may be lighter or
heavier than the raffinate and so the extract may be shown coming from the top of the
equipment in some cases and from the bottom in others. The operation may be repeated if more
than one contact is required but when the quantities involved are large and several contacts are
needed, continuous flow becomes economical. Figure shows the separating funnel used in
liquid - liquid extraction process to separate the components of a mixture into two immiscible
solvent phases of different densities.
Fig. Separating Funnel
37
Utilities required
Beaker, Burette, Funnel, Separating funnel, Distilled Water, 15% Acetic Acid solution, Ethyl
Acetate, Phenolphthalein, 0.1 N NaOH solution, Stopwatch
EXPERIMENTAL
Experiments were conducted to find out the number of stage required for the extraction of
acetic acid by ethyl acetate and consequently extraction isotherm were plotted.
PROCEDURE
1. Experiments were performed to find out optimum time required for maximum
extraction percentage in extraction of acetic acid by using ethyl acetate at equal
volume ratio.
2. Take a known amount (volume) of Ethyl Acetate having initial concentration Ci and
keep it in the separating funnel.
3. Take same amount of ethyl acetate nd mix it with the acetic acid solution in the same
separating funnel.
4. Mix it thoroughly for 1min.
5. Keep the separating funnel on the stand for the separation of two different layers.
6. Lower layer (extract) is separated from the raffinate and 10 ml of the sample is taken
for titration.
7. Titrate the sample with 0.1N NaOH with phenolphthalein indicator.
8. Repeat the experiment for different mixing time.
Material Balance
Figure shows stream “S” (solvent) and “A” (aqueous) are mixed for the sufficient time with
S/A ratio “r”. Initial and final concentration of solvent is S1 and S2 and that of aqueous is A1
and A2.
𝐴2
Equilibrium concentration S2 and A2 are related as 𝑆2 = 𝑆1 − . It can be noted that here A1
𝑟
=0
A1
S1 A1
S2
S/AS=1 r Time =2min
A2
38
OBSERVATION
Observation table
Sr No Time Volume of Volume of Sample (ml) Readings
extract (ml) Raffinate (ml)
(ml)
CALCULATION
V = volume of raffinate
S = volume of sample
V = burette reading
Total amount of acetic acid in sample
N1. V = N2. S
N2 = (N1.v)/S
For acetic acid normality = molarity
Mass of acetic acid raffinate = (V*N2*mol wt)/ 1000
𝑤𝑡. 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑
% 𝐸𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 = ∗ 100
𝑖𝑛𝑡𝑖𝑎𝑙 𝑤𝑡 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑
Similar calculation were done for all experiments performed at different time.
Further applying material balance find the concentration S2 which is related with A2 by
equation
S2 = S1 – A2
Calculation table
Sr. No Time % Extraction A2 (mole/lit) S2 (mole/lit)
39
1. Interface should not be disturbed during the experiment.
2. Always use clean water & ensure that there are no foreign particles in it.
3. Never use feed tanks to store the chemicals used in the experiment.
40
EXPERIMENT- 10
LIQUID LIQUID EXTRACTION
(Phase ratio)
OBJECTIVE:
To study the effect of phase ratio on extraction of acetic acid (dispersed phase) by ethyl
acetate (continuous phase).
To establish equilibrium isotherm between concentration of acetic acid and ethyl acetate.
THEORY
41
Utilities required
Effect of S/A (solvent to aqueous) ratio
 Experiments were performed for the extraction of acetic acid in toluene by using ethyl
acetate at different S/A ratio and extraction time was kept constant for 2min.
 Take a known amount (volume) of Ethyl Acetate having initial concentration Ci and
 Take same amount of ethyl acetate and mix it with the acetic acid solution in the same
separating funnel.
 Mix it thoroughly for 2 min.
 Keep the separating funnel on the stand for the separation of two different layers.
 Lower layer (extract) is separated from the raffinate and 10 ml of the sample is taken
for titration.
 Titrate the sample with 0.1N NaOH with phenolphthalein indicator.
 Repeat the experiment for different S/A ratio.
Extraction isotherm
Extraction isotherm was plotted by assuming perfect equilibrium between the raffinate and
extract phase at each stage. Figure shows the systematic of the stage wise batch extraction
stream “S” (solvent) and “A” (aqueous) are mixed for the sufficient time with S/A ratio “r”.
Initial and final concentration of solvent is S1 and S2 and that of aqueous is A1 and A2.
𝐴2
Equilibrium concentration S2 and A2 are related as 𝑆2 = 𝑆1 − . It can be noted that here A1
𝑟
= 0.
A1
S1 A1
S2
S/AS=1 r Time =2min
A2
42
OBSERVATION
Observation table
Sr Time Volume of Volume of Sample (ml) Readings (ml)
No extract (ml) Raffinate (ml)
1
2
3
4
CALCULATION
V = burette reading
N1. V = N2. S
N2 = (N1.v)/S
Similar calculation were done for all stages of experiments performed.
𝐴2
Outlet equilibrium concentration are related as 𝑆2 = 𝑆1 − 𝑟
CALCULATION TABLE
Sr. Time % Extraction A2 (mole/lit) S2 (mole/lit)
No
From different values of S2 and An construct isotherm on normal graph
43
Experiment- 11
LIQUID LIQUID EXTRACTION
(Number of stages)
OBJECTIVE:
 To find out the number of stages required for extraction of acetic acid (dispersed
phase) by ethyl acetate (continuous phase).
 To establish equilibrium isotherm between concentration of acetic acid and ethyl
acetate.
THEORY
44
Utilities required
To find the number of stage required for complete extraction
1. Experiments were performed to find out optimum time required for maximum
extraction percentage in extraction of acetic acid by using ethyl acetate at equal
volume ratio and extraction time was kept constant for 2mins.
2. Take a known amount (volume) of Ethyl Acetate having initial concentration Ci and
3. Take same amount of ethyl acetate and mix it with the acetic acid solution in the same
separating funnel.
4. Mix it thoroughly for 2 min.
5. Keep the separating funnel on the stand for the separation of two different layers.
6. Lower layer (extract) is separated from the raffinate and 10 ml of the sample is taken
for titration.
7. Titrate the sample with 0.1N NaOH with phenolphthalein indicator.
8. Repeat the experiment by taking fresh solvent and same raffinate until acetic acid is
completely extracted.
Extraction isotherm
Extraction isotherm was plotted by assuming perfect equilibrium between the raffinate and
extract phase at each stage. Figure shows the systematic of the stage wise batch extraction
stream “S” (solvent) and “A” (aqueous) are mixed for the sufficient time with S/A ratio = 1.
S0 and S1, S2 are Initial first and second stage concentration of solvent and that of aqueous
phase concentration are A0, A1 and A2 respectively.
𝐴2
Equilibrium concentration S2 and A2 are related as 𝑆2 = 𝑆1 − . It can be noted that here
𝑟
A0 =
A0
S0 A1
S1
S1 1st stage
A1
T
S0 2nd stage S2
45
A2
OBSERVATION
Observation table
Sr No Time Volume of Volume of Sample (ml) Readings
extract (ml) Raffinate (ml)
(ml)
1
2
3
4
CALCULATION
V = burette reading
N1. V = N2. S
N2 = (N1.v)/S
Similar calculation were done for all stages of experiments performed.
Outlet equilibrium concentration are related as
First stage S1 = S0 – A1
Second stage S2 = S0 – A2
CALCULATION TABLE
Sr. No Time % Extraction An (mole/lit) S2 (mole/lit)
From different values of Sn and An construct isotherm on normal graph
46
PRECAUTIONS AND MAINTENCE INSTRUCTION

Don’t exceed the pressure above 1kg/cm2
47
Experiment- 12
LIQUID-LIQUID EXTRACTION IN A PACKED BED
OBJECTIVE:
1. To study the extraction of acetic acid from water by ethyl acetate (continuous phase) in a packed
bed column.
2. To determine the overall mass transfer coefficient based on continuous phase.
3. To determine the overall height of transfer unit based on continuous phase.
INTRODUCTION:
Liquid- 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 distribute themselves differently between the two liquid phases, a certain degree of separation
will results, and this can be enhanced by use of multiple contacts or their equivalent in the manner of
gas absorption and distillation.
THEORY:
Packed towers filled with some random packing (say rasching rings) are widely used for extraction of
valuable chemicals from dilute solutions by liquid-liquid extraction. The packing provides a larger
extract 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 the liquid phases in the tower. For dilute solutions and where the equilibrium relation is
straight line, a simple expression can be obtained for determining the required height of a column (Z).
………………… (1)
Where LT, CT, C*T and KTa are volumetric flow rate, concentration of extract material, concentration
of extract material at equilibrium and overall mass transfer coefficient in dispersed phase.
48
Where CT1, CT2, CT1, CT2 CT LM (∆ ) are inlet, outlet concentration, concentration difference at inlet,
concentration at outlet and log mean concentration difference in dispersed phase. The overall mass
transfer coefficient based on dispersed phase , KTa is defined as:
Where L’T is molar flow rate of solution, V is volume of packing. Similarly overall mass transfer
coefficient based on continuous phase (water), KWa is defined as:
Where L’w is Malor flow rate of water.
The tower performance is generally based on extraction rate data and evaluated in terms of overall
height of transfer unit, based on continuous phase, HOW and the extraction factor expressed in terms
of flow rate ratios of the liquid phases,
Where, m is the slope of equilibrium curve, m = dCW/dCT Under certain conditions (e.g. low
concentrations) m is a constant As per chilton and colburn, the over all height of transfer unit based on
continuous phase (water), HOW is defined as:
And the over all height of transfer unit based on dispersed phase (toluene),
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:
Plot the graph of HOW vs × m(Qw/ QT) m on a simple graph and calculate the slope HT and intercept HW.
Where HW and HT are the individual height of transfer unit in continuous and dispersed phase
49
DESCRIPTION:
The set up consists of a glass column packed with rasching rings. Rotameters are provided to measure
the flow rate of solvent and solute. Two feed tanks are given with pump for feed supply. Pressure gauge
and pressure regulator are provided to measure the pressure. Two receiving tank are given to collect
extract and raffinate phase product.
Starting procedure
1. Prepare a solution of Acetic acid and water by mixing 10 to 15% acetic acid in 20 liter of water.
2. Take 20 liter of Ethyl acetate.
3. Fill one burette by 0.1N sodium hydroxide solution.
4. Close all the valves V1-V10.
5. Fill the one feed tank with prepared solution and other with ethyl acetate.
6. Connect compressed air supply to the set-up at the valve V10.
7. Open valve V10 and set air pressure 1.0 to 2.0 kg/cm2 by pressure regulator and pressure gauge.
Open the valve V3-V4 and fill mixture solution in feed the tank A.
8. Close the valve V3-V4.
9. Also open the valve V5-V6 and fill water in the feed tank B.
10. Close the valve V5-V6.
11. Open and adjust the flow control valve V1-V2 for dispersed and continuous phase to same flow
rate values.
12. Wait till steady state achieves (approx 20 to 30 minute).
13. Collect the known amount of sample in measuring cylinder from both the outlet and note down
the volume of sample.
14. Titrate the sample solution of dispersed phase, against 0.1N sodium hydroxide in alcohol (add
NaOH from burette) by using phenolphthalein as an indicator.
15. Repeat the experiment for different flow rate of feed mixture and water.
Closing procedure
1. When experiment is over stop the flow of feed by close the valve V1-V2.
2. Reduce air pressure to 0 kg/cm2 by pressure regulator and pressure gauge.
3. Drain the packed column and feed tanks by open the valve V7-V9.
EQUIPMENT DATA
 Diameter of column Dc = 0.048 m
 Packed height of column Z = 0.75 m
 Weight of Acetic acid in feed solution WB = ____ gm
 Volume of Ethyl acetate in feed solution V = ____ Lit
 Normality of NaOH used to titrate the sample of dispersed phase N2 =
 Normality of NaOH used to titrate the sample of continuous phase N1 =
 Inlet concentration of benzoic acid in continuous phase CW 2 = k mole/m3.
50
CALCULATIONS:
Plot the graph of CW vs CT of equilibrium data and find the slope ‘m’.
S. No QT (LPH) QW m KTa KWa HOT (m) HOW (m)

(LPH) (QW/QT) (kmole/m3 (kmole/m3
sec(kmole/m3 sec
)) (kmole/m3
))
Plot the graph of HOW vs m×(Qw/QT) on a simple graph and calculate the slope HT and intercept HW.
BLOCK DIAGRAM
51
Plot the graph of HOW vs m×(Qw/QT) on a simple graph and calculate the slope HT and intercept HW.

1. Interface should not be disturbed during the experiment.
2. Don’t exceed the flow rate more than 15 LPH.
3. Water outlet should be toluene free.
4. Always use clean water & ensure that there are no foreign particles in it.
5. Always clean the column feed tanks & receiving tanks properly after experiment.
6. Never use feed tanks to store the chemicals used in the experiment.
7. Always drain the column once before running the experiment on desired second flow rates.
52
Experiment- 13
STEAM DISTILLATION
OBJECTIVE:
To study the steam distillation process using turpentine oil as a feed stock.
 To calculate the vaporizing efficiency of the stem distillation column.
 To calculate the percentage recovery of turpentine oil.
INTRODUCTION:
Steam distillation is a separation process in which live steam is blown through a liquid
containing a component. When the component vaporizes slowly and leaves with the steam. The
component is the target component which we want to recover reasonably pure state. The
mixture to be separated may contain traces of a non-volatile impurity.
The feed is taken in the distillation vessel or still through which live steam is sparged at the
bottom. The vapour containing the vaporized product as well as steam is led to a condenser. If
the component has only little miscibility with water, the condensate forms two layers and can
be easily separated to recover to product.
THEORY:
If the substance A is immiscible with water. The feed contains A and traces of non-volatile
impurities. Let PAv be the vapour pressure of A at the operating temperature, PBv the vapour
pressure of B (water), and P be the total pressure. Since A & B are essentially immiscible, the
total pressure is the sum of the individual pressure
𝑷 = 𝑷𝒗𝑨 − 𝑷𝒗𝑩
If mA moles of the substance are volatilized out by putting in mB moles of steam and if the system
operates at equilibrium, we may write:
𝑀𝐴 𝑃𝐴𝑣 𝑃𝐴𝑣
= 𝑣 =
𝑀𝐵 𝑃𝐵 𝑃 − 𝑃𝐴𝑣
However, if the system does not operate at equilibrium, the partial pressure of A will be less than
its vapour pressure. To take into account such a deviation, we define a factor called vaporizing
efficiency E of the product such that the partial pressure of A in the steam phase is
P𝐴 = EP𝐴𝑣
P M𝐴
E = 𝑣( )
P𝐴 𝑀𝐴 + 𝑀𝐵
53
DESCRIPTION:
The set-up consists of jacketed pressure vessel. Steam generator is provided to generate the steam.
Condenser is given to condensate the vapour. Rotameter is provided to measure the flow rate.
Steam trap is for releasing the pressure. Digital temperature indicator & digital temperature
controller are provided to indicate and control the temperature.
UTILITIES REQUIRED:
 Electrical Supply: Single Phase, 220 V AC, 50 Hz, 32 Amp MCB with earth connection.
 Water Supply: Continuous @ 2 LPM at 1 bar.
 Turpentine oil : 2 Lit.
STARTING PROCEDURE:
1. Take known amount of turpentine oil and note down the volume of it.
2. Take known amount of water, note down the volume of it & mix it with turpentine oil.
4. Ensure that ON/OFF switches given on the panel are at OFF position.
5. Fill water in the steam generator by open the valve V1 and air vent valve V2 and close
them.
6. Charge the distillation still with turpentine oil & water mixture by open the valve V6 and
air vent valve V7.
7. Switch ON the main power supply.
8. Set the temperature of steam generator with the help of DTC (approx. 115C).
9. Switch ON the heater.
10. Wait for the steam formation.
11. As steam formed, open the steam supply valve V3.
12. Start the supply of steam in jacket by open the valve V4 and air vent valve V9.
13. When the temperature in the still reaches 2C below the distillation temperature, stop the
supply of steam in jacket by close the valve V4.
14. Start the flow of live steam by open the valve V5.
15. Connect cold water supply to condenser.
16. Note down the live steam pressure.
17. Collect the condensed vapors in glass separating chamber.
18. Continue the distillation process for sufficient time (approx 1 hr).
19. Stop the steam supply and collect the distillate in separate chamber.
20. Wait for the formation of two layers.
21. Collect the separate formed layers by open the valve V8 & weigh them
CLOSING PROCEDURE:
1. When experiment is over stop the water supply.
2. Switch OFF the heater.
3. Switch OFF the main power supply.
4. Drain the vessel by open the valve V10.
5. Drain the steam generator by open the valve V11.
54
OBSERVATION & CALCULATION
 Molecular weight of turpentine oil MA = 136 g/mole
 Molecular weight of water MB = 18 g/mole
P0 = kg/cm2
T = 0C
VA = lit.
VB = lit.
VAD = lit.
CALCULATIONS
To calculate the property of turpentine oil ρA and ρB for water at Temperater T
ρA = Kg/m3
ρB = Kg/m3
To calculate the antion constant of turpentine oil (A, B, C) at temperature T (oC) from data book.
P = 735.74×P0 (mm of Hg)
ρ𝐴 𝑉𝐴
𝑊𝐴 = kg
1000
ρ𝐵 𝑉𝐵
𝑊𝐵 = kg
1000
ρ𝐴 𝑉𝐴𝐷
𝑊𝐴𝐷 =
1000
P M𝐴
E = 𝑣( ) × 100
P𝐴 𝑀𝐴 + 𝑀𝐵
𝑊𝐴𝐷
𝑅 = × 100
𝑊𝐴
55
PRECAUTION & INSTRUCTIONS:
1. Never run the apparatus if power supply is less than 180 volts & more than 230 volts.
2. Don’t switch ON the heater before filling water in the steam generator.
3. For condenser the cold water supply should be constant.
4. Feed should be fill-up in the vessel at least up-to the mark.
BLOCK DIAGRAM
56
Experiment- 14
VAPOUR LIQUID EQUILIBRIUM
OBJECTIVE
To study the vapor liquid equilibrium curve
 To plot the vapor-liquid equilibrium curve for water methanol mixture
INTRODUCTION:
The design of distillation and other contacting equipment requires reliable VLE data. It shows
the relationship between the composition of the vapor and that of liquid in equilibrium with the
vapor for a binary mixture at constant pressure or constant temperature. Although relatively
few ideal solutions are known whose equilibrium relations can be calculated from vapor
pressure – temperature data of the pure components, by far the larger numbers of systems of
industrial importance are non-ideal; and attempts to predict the equilibrium compositions of
such mixtures from theoretical considerations alone have not proved successful. It has been the
practice to determine such data experimentally under various conditions.
THEORY:
Vapor liquid diagram shows relationship between the composition of the vapor and that of
liquid in equilibrium with the vapor for a binary mixture at constant pressure or constant
temperature. The basic data of any distillation problem are the equilibrium between the liquid
and vapour phases of the system subjected to distillation. Hence is of great importance to study
the vapour-liquid equilibrium.
Theoretical VLE curve can thus be calculated by choosing various boiling points of the mixture
and calculate x and y. Carbon tetrachloride and toluene system closely follows ideal behavior.
DESCRIPTION:
The set-up consists of distillation still with a heating element. An electrical dimmer stat is
connected to heating element for varying heat input. The vapours form the top of column are
condensed in the concentric tube type condenser by circulating cooling water. The condensate
is feedback to column as reflux. A tank with pump is provided to circulate cold water to
57
condenser. Flow rates can be regulated through control valve fitted. Instrumentation is done to
measure the temperatures at different points
UTILITIES REQUIRED:
Electrical Supply: Single Phase, 220 V AC, 50 Hz, 5-15 Amp combined socket with earth
connection.
Water Supply (Initial fill)

Floor Drain Required.
 Refractrometer.
 Carbon
tetrachloride/water : 500 ml
 Toluene/methanol : 1 Lit
STARTING PROCEDURE:
1. Prepare solution of 100ml methanol and 400 ml water.
3. Ensure that switches given on the panel are at OFF position.
4. Fill water in the water tank.
5. Charge the feed solution in the distillation still by open the funnel valve V1.
6. Switch ON the power supply.
7. Switch ON the heater.
8. Gradually increase the dimmer stat and observe temperature.
9. When temperature starts increasing switch ON the pump.
10. Open the valve V2 and by-pass valve V3 and allows cooling water to pass through the
condenser
11. Maintain temperature above 70 and below 100 oC by using PID controller.
12. After observing constant temperature collect sample of distillate by open the valve V4.
13. Repeat the experiment for different feed mixture. (Increase the composition of
methanol)
CLOSING PROCEDURE:
1. Experiment is over switch OFF the pump.
2. Switch OFF the heater.
3. Switch OFF the main power supply.
4. Drain the vessel by open the valve V5.
5. Drain the water tank by open the valve V6
58
OBSERVATION & CALCULATION
DATA:
Total Pressure Po 1.033 Kg/Cm2
Constant A 16.017
Constant B 2696.25
Constant C 226.24
X
RI
OBSERVATION TABLE
S.No. T oC R.I
CALCULATION
P = Po × 105 (N/m2)
x=
CALCULATIOPN TABLE-1
S,No T oC x
𝐵
𝑃𝐴𝑂 = 𝑒 𝐴−𝐶+𝑇
𝑃𝐴 = 𝑃𝐴𝑜 × 133.3
𝑃𝐴 𝑥
𝑦 =
𝑃
59
CALCULATION TABLE:-2
S.No. T x y
 Plot T vs (x,y) on a simple graph.

 Plot x vs y on a simple graph

1. Fill the vessel atleast half of the capacity.
2. Drain the vessel and water tank after completion of the experiment.
3. Don’t run the pump before filling the tank with water.
4. Don’t start the heater before filling the chemicals into the still
BLOCK DIAGRAM
60
Experiment- 15
BUBBLE CAP DISTILLATION COLUMN

OBJECTIVE:
To study the operation of bubble cap distillation column.
AIM:
1. To verify the Rayleigh equation
2. To obtain the T-x data under total reflux condition at steady state and compare it with
theoretical value
3. To operate the column under total reflux condition and calculation the minimum
number of theoretical stages using Fenske’s equation
4. To operate the column under any desired reflux condition and calculate theoretical
number of stages using McCabe Thiele’s method
5. To calculate the overall efficiency of the bubble cap distillation column
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.
When distillation is carried out in plate columns in which each plate constitutes a single stage.
The number of theoretical stages required to effect a required separation. There are so many
types of tray. The main requirement of the tray is that it should provide intimate mixing
between the liquid and vapour streams.
The bubble cap tray has been the most widely used tray because of its range of operation but it
is now tending to be superseded by newer types, such as the valve tray. The individual caps are
mounted on risers and have rectangular or triangular slots cut around their sides.
THEORY:
Part-1
Bubble cap distillation column are capable of dealing with very low liquid rates and are
therefore useful for operation at low reflux ratios.
For simple batch distillation process, initially the still is filled with F moles of feed with x F as
the mole fraction of the more volatile component. Let at any moment the number of moles of
liquid in the still be B having a mole fraction x of the more volatile component and let the
moles of accumulated condensate be D. concentration of the equilibrium vapour is y*. Over a
small time, the change in the amount of liquid in the still is dB and the amount of vapour
withdrawn is dD. The following differential mass balance equations may be written:
Total material balance:
61
-dB = dD ………………………….. (1)
Component A balance:
-d(Bx) = y* dD …………………………. (2)
On solving the above equation:
-Bdx – xdB = y* dD
Put –dB = dD from eqn (1):
- Bdx = y* dD – xdD
- Bdx = (y* - x)dD
Again put dD = -dB
Bdx = (y* - x) dB ………………………..(3)
By arranging the above equation:
𝑑𝐵 𝑑𝑥
= ………………………… (4)
𝐵 (y∗ − x)
Integrating eqn (4)

𝐵 𝑑𝐵 𝑥 𝑑𝑋
∫𝐹 = ∫𝑋 𝐵 𝑦 ∗ −𝑥 …………………………..(5)
𝐵 𝐹
Eq.(5) is the Rayleigh equation, which describes the variation of the liquid are vapour mole
fraction, x,y in terms of the fraction remaining in the still.
𝐹 𝑋 𝑑𝑋
𝑙𝑛 𝐵 = ∫𝑋 𝐹 𝑦 ∗ −𝑥 ………………………….(6)
𝐵
We have:
𝛼𝑋
𝑦 ∗ = 1+(𝛼−1)𝑋 ………………………. (7)
For constant relative volatility𝛼, we can write the equation (6):

𝑋𝐹
𝐹 𝑑𝑋
𝑙𝑛 = ∫
𝐵 𝛼𝑋
𝑋𝐵 −𝑋
1 + (𝛼 − 1)𝑋
𝐹 𝑋 𝑑𝑋 𝑑𝑋
𝑙𝑛 𝐵 = ∫𝑋 𝐹 (𝛼−1)𝑋(1−𝑋) + (1−𝑋) ……..…………………….(8)
𝐵
By partial differentiation of the above equation:

𝐹 1 𝑋𝐹 (1 − 𝑋𝐵 ) (1 − 𝑋𝐵 )
𝑙𝑛 = [𝑙𝑛 ] + 𝑙𝑛 [ ]
𝐵 𝛼−1 𝑋𝐵 (1 − 𝑋𝐹 ) (1 − 𝑋𝐹 )
𝐹 (1 − 𝑋𝐵 ) 1 𝑋𝐹 (1 − 𝑋𝐵 )
𝑙𝑛 − 𝑙𝑛 [ ]= [𝑙𝑛 ]
𝐵 (1 − 𝑋𝐹 ) 𝛼−1 𝑋𝐵 (1 − 𝑋𝐹 )
62
𝐹(1 − 𝑋𝐹 ) 1 𝑋𝐹 (1 − 𝑋𝐵 )
𝑙𝑛 [ ]= [𝑙𝑛 ]
𝐵(1 − 𝑋𝐵 ) 𝛼−1 𝑋𝐵 (1 − 𝑋𝐹 )
𝐹(1 − 𝑋𝐹 ) 𝑋𝐹 (1 − 𝑋𝐵 ) 𝐹(1 − 𝑋𝐹 )
𝛼𝑙𝑛 [ ] = [𝑙𝑛 ] + 𝑙𝑛 [ ]
𝐵(1 − 𝑋𝐵 ) 𝑋𝐵 (1 − 𝑋𝐹 ) 𝐵(1 − 𝑋𝐵 )
𝐹(1 − 𝑋𝐹 ) 𝐹𝑋𝐹
𝛼𝑙𝑛 [ ] = 𝑙𝑛 [ ]
𝐵(1 − 𝑋𝐵 ) 𝐵𝑋𝐵
The above equation is more convenient from of Rayleigh equation.
Batch distillation with only a single still does not give a good separation unless the relative
volatility is very high. To obtain product with a narrow composition range, a rectifying 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 analysed using the same operating
line equation as for the rectifying section of the continuous distillation:
𝑅 𝑋𝐷
𝑦𝑛+1 = 𝑋𝑛 +
𝑅+1 𝑅+1
For the binary system:
Y2 = 1- y1
X2 = 1- X1
Since the slope of the operating line is R / (R+1), the slope increases as the reflux increases
until when reflux is infinite. Under total reflux slope is 1. The operating line then coincides
with the diagonal. The number of plate is minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration of XB
and XD based on the relative volatility of the components α, which is defined in terms of
equilibrium concentrations:
Minimum number of theoretical plates required:
𝑙𝑜𝑔[𝑋𝐷 (1−𝑋𝐵 )/𝑋𝐵 (1−𝑋𝐷 )]
𝑁𝑚 = −1 …………(10)
𝑙𝑜𝑔𝛼
The above equation is known as Fenske’s eqn.

The final ratio does not change much over the range of temperature encountered in a typical
column, so the relative volatility is taken as constant.
Method to calculate number of theoretical plates (Mc-Cabe Thiele’s method):
Part-II
For the determination of theoretical plates at desired reflux ratio. We are using graphical
method which is called Mc-Cabe Thiele’s method.
63
In this method draw the equilibrium data on x-y plane. Locate the point xD,xB and xF on
diagonal. For the given reflux ratio R calculate the intercept on the rectifying section operation
line on the y-axis.
𝑥𝐷
𝐼=
𝑅+1
Now calculate the slope of the feed line:

𝑞
𝑆 = tan−1 ( )
𝑞−1
Where q is the fraction of liquid in the feed.
Fellow the following procedure to calculate theoretical number of plates (Nt):
a) Plot the equilibrium data on x-y plane.
b) Locate the point xD, xB, and xF on diagonal.
c) Draw the rectifying line from point xD with intercept I on the y axis
d) Also draw the feed line from the point xF with slope S and intersect the rectifying line,
that intersection point is M.
e) Now draw the stripping line from point xB to the intersection point M.
f) Draw horizontal line from the point xD to equilibrium curve.
g) Draw vertical line from the point at equilibrium curve (where horizontal line is end) to
the operating line.
h) The above step made triangle construction
i) Again draw horizontal line from the point at operation line (where vertical line is end)
to the equilibrium curve
j) Repeat the above three steps between equilibrium curve and operating line, till cover
the point xB on diagonal
k) Count the number of triangles made
l) Number of triangles is equal to number of theoretical stages including reboiler
m) Subtract one from the number of triangle, and then it is theoretical number of stages
required at desired reflux conditions
For the overall efficiency of the column can be used in following formulas:
𝑁𝑡
𝜂0 = ∗ 100 (%)
𝑁𝐴
Where NA is number of actual plates in the column
DESCRIPTION:
The set-up consists of a column with seven plates for mounting the bubble caps. Each cap
is provided with one bubble cap. An electrically heated reboiler is installed at a bottom of
the column. Steam generator is provided to generate the steam. A tank is provided to collect
64
the bottom product. Shell and tube type condenser is provided to condensate the vapour. A
tank with pump and rotameter is provided for circulating of cooling water. Reflux drum is
provided to collect the condensate. Receiving tank is for collecting the distillate. Drain
valves are provided for drainage purpose.
UTILITIES REQUIRED:
1. Electrically supply : single phase,220 V AC, 50 Hz, 32 Amp MCB with earth
connection.
2. Water supply: continuous @ 2 LPM at 1 bar
3. Refractometer for analysis
Starting procedure:
1. Prepare calibration chart of refractive index and liquid composition of methanol
2. Prepare methanol-water solution by mixing known amount of distilled water and
methanol (composition of methanol in solution should be in the range of 15 to 25% by
volume)
3. Measure the refractive index of feed solution
4. Note down the volume of methanol
5. Close all the valves V1-V13
6. Ensure that ON/OFF switches given on the panel are at OFF position
7. Fill vessel with methanol-water solution by open the funnel valve V1 and air vent valve
V2
8. Close the funnel value V1 and the air vent valve V2
9. Switch ON the main power supply
10. Set the temperature of solution above boiling point of methanol but less than 100 0C by
the DTC
11. Switch ON the heater
12. Switch ON the cyclic timer and set the total reflux condition
13. Open the air vent valve V10 provided at the top of condenser and after observing vapour
coming out of it close the valve V10
14. Switch ON the pump and set the condenser cooling water flow rate by adjust the valve
V12
15. Wait till required temperature or steady state condition achieves
16. Note down the temperature of each tray
17. Now take out the samples from each tray by open the valve V3-V9
18. Also collect the distillate and bottom product by open the valve V11 and V13 respectively
19. Cool down the samples to room temperatures & measure their refractive indices
20. Now adjust the cyclic timer to a desired reflux ration & wait for steady state
21. Note down the temperatures of each tray
22. Now take out the samples from each tray by open the valve V3V9
23. Also collect the distillate and bottom product by open the valve V11 and V13 respectively
24. Cool down the samples to room temperature & measure their refractive indices
25. Repeat the experiment for different set point temperatures and reflux rations
Closing procedure:
65
1. When experiment is over switch OFF the heater
2. Switch OFF the main power supply to the set-up
3. After 10 min stop the water supply
4. Drain the vessel after temperatures fall down to atmospheric values by open the valve
V13
OBSERVATION & CALCULATION:

Data: 1
Relative volatility α = 3.32
Molecular weight of methanol MM = 32 g/mole
Molecular weight of water MW = 18 g/mole
Actual number of plates NA = 7
Enthalpy of feed HF = 0 KJ/mole
Data: 2
x R.I(at 25°C)
0 1.33
0.1 1.3315
0.2 1.3325
0.3 1.3345
0.4 1.336
0.5 1.337
0.66 1.3375
0.75 1.337
0.8 1.3345
0.9 1.3305
1 1.3235
T-x-y data for methanol water

Y-Values system
T(°C) X1 Y1 X1 Y1
1.34
(RI) (RI)
1.338 369 0.0084 0.103
365 0.0258 0.227
1.336
360 0.0680 0.391
1.334 353 0.1370 0.568
349 0.2400 0.680
1.332
343 0.4800 0.790
1.33 341 0.5720 0.820
339 0.7410 0.906
1.328
1.326
1.324
1.322
0 0.2 0.4 0.6 0.8 1 1.2
66
Observation (At Total Reflux Condition):
R = ………………..
V = ……………….. Lit
TF= ………………. °C
R.IF =……………..
R.IB =………………
R.ID =………………..
Observation Table (At Total Reflux Condition):
S.NO T(°C) R.I
1
2
3
4
5
6
Observation (At Desired Reflux Condition):

R = ………………..
TF= ………………. °C
R.IF =……………..
R.ID =………………..
Observation Table (At Desired Reflux Condition):

S.NO T(°C) R.I
1
2
3
4
5
6
Calculations (At Total Reflux Condition):

X = ……………………. [from R.I vs x graph]
67
Calculation Table :1
S.NO T(°C) x xthe
1
2
3
4
5
6
7
XF =………………………. [From R.I vs x graph, value of x corresponding to R.IF]

XB =………………………. [From R.I vs x graph, value of x corresponding to R.IB]
XD =………………………. [From R.I vs x graph, value of x corresponding to R.ID]
To calculate the property of methanol(ρ) at temperature TF (°C) from data book.
ρ=………………………..(kg/m3)
𝜌∗𝑉
𝐹= (𝑘𝑚𝑜𝑙)
𝑀𝑀 ∗ 1000
𝑋𝐹 − 𝑋𝐷
𝐵= ∗ 𝐹 (𝑘𝑚𝑜𝑙)
𝑋𝐵 − 𝑋𝐷
𝐹 𝑋𝐹
𝑙𝑛 [ ] = ⋯ … … … … … … ..
𝐵 𝑋𝐵
𝐹(1 − 𝑋𝐹 )
𝛼 ln = ⋯…………….
𝐵(1 − 𝑋𝐵 )
𝐹 𝑋𝐹 𝐹(1 − 𝑋𝐹 )
𝐸 = 𝑙𝑛 [ ] − 𝛼 ln
𝐵 𝑋𝐵 𝐹(1 − 𝑋𝐹 )
𝑋𝐷 (1 − 𝑋𝐹 )
𝑙𝑛 [ ]
𝑋𝐵 (1 − 𝑋𝐵 )
𝑁𝑚 = −1
ln 𝛼
Calculations (At Desired Reflux Condition):
XF =……………………[From R.I vs x graph, value of x corresponding to R.IF]
XD =……………………[From R.I vs x graph, value of x corresponding to R.ID]
X = …………………… [From R.I vs x graph]
Calculation table: 2
S.NO T(°C) x
1
2
3
68
4
5
6
7
𝛼𝑥
𝑦=
1 + (𝛼 − 1)𝑥
S.NO T(°C) x y
1
2
3
4
5
6
7
Plot T vs (x,y) on a simple graph

TD = ………(°C)[corresponding value of T with respect to xF from T-y curve]
TB = …….…(°C)[corresponding value of T with respect to xB from T-x curve]
To calculate the property of methanol (CPM, λM) and water (CPM, λW) at temperature TB (°C)
from data book
CPM =………………………….(kJ/kg °C )
CPW=………………………….(kJ/kg °C )
λM = …………………………. (kJ/kg)
λW = …………………………. (kJ/kg)
𝐶𝑃𝐹 = 𝑥𝐹 𝐶𝑃𝑀 + (1 − 𝑋𝐹 )𝐶𝑃𝑊 (kJ/kg °C)
𝑀𝑎𝑣 = 𝑋𝐹 𝑀𝑀 + (1 − 𝑋𝐹 )𝑀𝑊
𝐻𝐿 = 𝐶𝑃𝐹 𝑀𝑎𝑣 (𝑇𝐵 − 𝑇𝐹 )(𝑘𝐽/𝑘𝑚𝑜𝑙)
𝐻𝐺 = [(𝑋𝐹 )[𝐶𝑃𝑀 𝑀𝑀 (𝑇𝐷 − 𝑇𝐹 ) + 𝜆𝑀 𝑀𝑀 ] + (1 − 𝑋𝐹 )[𝐶𝑃𝑊 𝑀𝑊 (𝑇𝐷 − 𝑇𝐹 ) + 𝜆𝑊 𝑀𝑊 ]]
𝐻𝐺 − 𝐻𝐹
𝑞=
𝐻𝐺 − 𝐻𝐿
𝑞
𝑆 = tan−1( )
𝑞−1
𝑋𝐷
𝐼=
𝑅+1
Nt =………………………. (Refer theory PART -II)
69
PRECAUTION & MAINTENANCE INSTRUCTION:

1. Heater should not be switched ON before filling the solution in reboiler.
2. Always drain tanks and reboiler when experiment is over.
3. Always use clean water and ensure that there are no foreign particles in the flow stream.
70
Experiment- 16
Drying
OBJECTIVE-
To find the rate of drying for a given porous/Nonporous material
INTRODUCTION
Drying is refer to the removal of small amount of water or organic liquids (e. g. organic solvent) from
solids (process materials). Dryer is a unit operation which liquid is separated from the solid by other
than mechanical means. This generally requires supplying heat, resulting in evaporation of liquid
The differences between drying and evaporation process drying process evaporation process Normally
carried out on solid material Normally carried out on liquid solution Remove relatively small of water
Remove large amount of water In most cases, involves the removal of water at the temperature below
its boiling point
APPLICATION OF DRYING
To eliminate moisture which may lead to corrosion and decrease the product stability To improve or
keep the good properties of material (e. g. flow ability, compressibility) To reduce the course of
transportation of large volume materials (liquid) To preserve the material (e. g. food products. ) To
make the material easy or suitable for handling As a final step in evaporation, filtration and
crystallization process.
Types of drying processes: Batch – the material is insert into the drying equipment and drying is
proceeds for a given period of time. Continuous – the material is continuously added to the dryer and
dried material is continuously removed. Types of drying physical conditions: Heat is added directly to
the air at atmospheric pressure and water vapor formed is remove by the air. Vacuum drying- Heat is
added indirectly by contact with a metal wall or by radiation and the water evaporated more rapid at
low pressure. Freeze drying- Water is sublimed from the frozen material
TYPES OF DRYER Tray / shelf dryer Suitable for lumpy or pasty solid The solid to be dried is spread
uniformly on a metal trays which can be loaded into the shelf or using the tray truck Steam-heated air
is recirculated by a fan over and parallel to the surface of the trays Yielding shorter drying times because
of the greater surface area exposed to the air
Drying process of a material can be described as a series of steps in which drying rate plays a key role.
Following figure shows typical drying rate curve for a constant drying conditions.
71
Point B represents equilibrium temperature conditions of the product surface. Section B to C of the
curve, known as the constant rate periods, represents removal of unbound water from the product. The
water acts as if the solid is not present. The surface of the product is very wet and water. And the water
activity is equal to one. The constant rate period continues as long as the amount of water evaporates is
equal to the amount of water supplied to the surface of the material.
The falling rate period is reached when the drying rate starts to decrease, and the surface water activity
falls to less than one. The rate of drying is governed by the internal flow of liquid or vapor. This point
is represented by C in the figure. At this point there is not enough water on the surface to maintain a
water activity value of one. The falling rate period can be divided into two steps. A first falling drying
rate occurs when wetted spots in the surface continually diminish until the surface is dried (Point D).
Second falling rate period begins at point D when the surface is completely dry. The plane of
evaporation recedes from the surface. Heat required for moisture removal is transferred through the
solid to the vaporization of moisture in the solid and the vapor moves through the solid into air stream.
The amount water removed in this period can be relatively small compared to the constant rate and first
falling rate period. However this period may take much longer than constant rate period because the
drying is slow.
Drying rate experiments can be simply done by measuring the weight change during drying. The
material to be dried is placed on the tray. The tray is suspended from a balance and exposed to air flow
in drying tunnel.
The following equation is used to calculate rate of drying:

Rate of drying = weight of water removed/weight of dry powder×time of drying × surface area
exposed.
72
Procedure
1. Switch on the power supply to the unit and press the ON/OFF key provided on the Panel.
2. Prepare the sample whose drying characteristics are to be determined by taking about 250gm-
500gm of material (usually sand, wet paper etc)
3. Fill the tray and spread the material evenly throughout the cross section of the tray.
4. Switch ON the blower and air flow
5. Switch ON the heater and adjust the Temperature of the Air by using digital temp controller
provided on the control panel.
6. After achieving a fairly high and stable Temperature note the temp and weight of the sample.
7. Repeat the steps for increasing temperature and note down the weight of the sample.
8. After certain time no loss of weight is observed for prolonged period of time switch OFF the
heater and note down the final weight of the sample.
9. Repeat the procedure by either varying the flow rate or take different sample for same
conditions and compare them with initial results.
Observation Table
S.No. Time Initial weight Final weight Initial temp. Final temp.
of Air of Air
1
2
3
4
Calculation
The drying time
Constant rate Time

𝑋0−𝑋𝑐
= 𝑡𝑐 =
𝑅𝑐
Falling rate time

𝑋0−𝑋𝑐 𝑋𝑐 𝑋𝑐
= 𝑡= + 𝑅𝑐 𝐼𝑛 𝑋2
𝑅𝑐
Results and Discussion

Plot the curve on graph by taking free moisture contain on x-axis and drying rate on y-axis. The curve
so obtained is called as drying rate curve.
73

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MASS TRANSFER

Department of Chemical Engineering

DOs and DON'Ts in the Laboratory

 Do thoroughly clean the glassware before and after use

Student Name: ABC

Student Id: XXBCH0XX

This is to certify that Mr/Ms …………………………………………………………

I/II in Jan-July/July-Dec 20… session.

Dr. Manish Kumar Sinha

Lab In-charge - MTO

This is to certify that Mr/Ms …………………………………………………………

Roll No ………………… of Fifth Semester, B. Tech., Chemical Engineering Department, SoT,

Lab – I/II in Jan-July/July-Dec 20… session.

Dr. Manish Kumar Sinha

Lab In-charge - MTO

3 Adsorption of acetic acid 11

6 Solid Liquid extraction 27

7 Water cooling tower 29

8 CO2 absorption in NaOH solution in Packed, Sieve plate and 34

9 Liquid Liquid extraction (effect of time) 38

16 Drying of Porous/Nonporous material 71

Amount of benzoic acid in feed = N1 * Eq. Wt * volume of feed = ……………… gm

Normality of benzoic acid in filtrate N1 = N2 V2 / V1

Amount of benzoic acid in filtrate = N1 * Eq. Wt * volume of filtrate (lit) = ……………… gm

Weight of crystals = amt. of B.Acid in filtrate

RESULT & CONCLUSION:

S. No. Mole fraction of A RI

S No. (1/(Y* - x)) x

 Physisorption ;-Physisorption is caused mainly by intermolecular forces(Van der

qeq= na / ms = f (Ceq) (1)

where qeq is the amount of adsorbate per unit mass of adsorbent.

The Freundlich isotherm

qeq= na / ms K. (Ceq)a (2)

where, na Amount of the adsorbate(grams) & ms = Amount of the adsorbent

In Eqn (2) K and a are constants.

The Langmuir Isotherm

𝜃 : Fraction of the solid surface covered by the adsorbed molecules

K: Adsorption equilibrium constant

Ceq: Equilibrium concentration

∅ = qeq / qmeq (4)

Hence Eqn 3 takes the form of

qeq / qmeq = K.( Ceq) /(1+K . Ceq) (5)

Ceq / q = Ceq / qmeq + 1/(K . qmeq ) (6)

Chemical :- Activated carbon, Acetic acid, Sodium Hydroxide, Phenolphthalein,

RESULTS AND CONCLUSION

PRECAUTION AND MAINTENANCE

SOLID IN AIR DIFFUSION

For component A (naphthalene) diffusing through non-diffusing B (air) at ambient temperature,

Then mass transfer coefficient can be calculated by following correlation:

Where Re is Reynolds number, Dp is diameter of the particle (naphthalene), V is velocity of

𝑆ℎ = 1.17𝑅𝑒 0.585 𝑆𝑐1/3 … … … … … … … … … … … … … … … … … … … … … … . (𝐶)

Kc is mass transfer coefficient

S. Flow rate (LPM) Molar flux Molar Partial Mass transfer

Alternative calculation for mass transfer coefficient

 Compare the value of Kc and Kp obtained by two different methods.

PRECAUTION & MAINTENANCE INSTRUCTIONS:

VAPOR IN AIR DIFFUSION

NA=XAN+JA=XA (NA+NB) + JA………………………….(1.1)

DAB is diffusivity coefficient of A diffusing in B. it is defined as the amount of mole of A

In case of steady state diffusion of A through stagnant B, NB = 0 equation 1.2 transforms to

Gentle flow of air

Amount (mole) of liquid diffuses in time interval “"∆𝑡" is given by