An Autonomous Institute

(Approved By AICTE, New Delhi Affiliated To

VTU, Belagavi Recognized By UGC
Under 2(f) & 12(B), Accredited By NBA &
NAAC)

DEPARTMENT OF CHEMICAL ENGINEERING

VI SEMESTER

MVJ21CH63 –MASS TRANSFER OPERATIONS LAB

ACADEMIC YEAR 2023–2024

LABORATORY MANUAL

NAM E OF THE STUDENT :

BRANCH :

UNIVERSITY SEAT NO. :

SEMESTER & SECTION :

BATCH :
Department of Chemical Engineering MVJCE

M.V.J. COLLEGE OF ENGINEERING

DEPARTMENT OF CHEMICAL ENGINEERING

VI SEMESTER

MVJ21CH63 – MASS TRANSFER OPERATIONS LAB

LABORATORY MANUAL

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Department of Chemical Engineering MVJCE
Department Vision:
Be a leading Chemical Engineering Department for quality technical education.
Department Mission:
1. Quality Teaching: - Provide high quality education in chemical and allied fields through
outcome based teaching –learning process.
2. Core competence:- Empower students and faculties to achieve proficiency in chemical
sciences and engineering using state-of-the-art laboratory facilities with modern technologies.
3. Centre of Excellence: Stimulate and encourage the pursuit of excellence in Chemical
Science and Engineering.
4. Skill Development:-Foster graduates with leadership qualities, entrepreneurship
skills, innovative thinking and professional ethics.

PROGRAM EDUCATIONAL OBJECTIVES (PEOS):

PEO1: Fundamentals: Graduates will apply chemical engineering principles in engineering
practice for employability in Chemical and allied industries.
PEO2: Higher Studies &Research: Graduates will pursue their post-graduation and
research in the fields of Chemical Engineering, Petrochemicals, Material Science,
Biotechnology, Nanotechnology, Environmental Engineering and allied areas.
PEO3: Entrepreneurship: Graduates will apply fundamental knowledge in chemical
engineering to nurture technologies for the benefit of humankind and to become successful
entrepreneurs.

PROGRAM OUTCOMES:
• Engineering Knowledge: Apply knowledge of mathematics and science appropriate to
Chemical Engineering discipline.
• Problem Analysis: Ability to identify, understand, formulate and solve chemical
engineering problems.
• Design/development of Solutions: An ability to analyze, design, implement, evaluate,
validate, Integrate and maintain a chemical process plant.
• Conduct investigations of complex objects: use research-based knowledge and research
methods including design of experiments, analysis and interpretation of data and synthesis
of the information to provide valid conclusions.
• Modern tool usage: An ability to use the techniques, skills, and modern engineering tools
necessary for chemical engineering practice.
• The Engineer and society: Use chemical engineering knowledge to solve social,
economic and environmental problems.

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Department of Chemical Engineering MVJCE
• Environment and sustainability: Understand the impact of the professional engineering
solutions in societal and environmental contexts and demonstrate the knowledge of and need
for sustainable development.

• Ethics: Understand professional, ethical and legal responsibilities.

• Individual and team work: Function effectively as a member or leader in diverse teams
and in multidisciplinary settings.

• Communication: Communicate effectively on complex engineering activities with

engineering community and with society at large, such as being able to comprehend and write
effective reports and design documentation, make effective presentations and give and receive
clear instructions.

• Management and finance: Demonstrate knowledge and understanding of the engineering

and management principles and apply these to one’s own work and as a member in a team.

• Lifelong learning: An ability to acquire new knowledge in computing discipline and

engage in lifelong learning.

PROGRAM-SPECIFIC OUTCOMES
PSO1: In-depth knowledge: Acquire in-depth knowledge of process calculations, transport
operations, reaction engineering, process control, economics, safety, and environmental
aspects required to work in diverse fields such as Petroleum refining, nano technology, food,
pharma, energy, environmental engineering etc.
PSO2: Computed aided Design: Solve Chemical engineering problems using
computational and simulation tools for design and optimization of chemical processes.

COURSE OUTCOMES
CO1: Determine the diffusivity of organic vapors in air using Arnold cell & Verify Himus
equation using surface evaporation.
CO2: Determine stage efficiency for Adsorption, Leaching & Extraction.
CO3: Estimate parameters affecting distillation using Simple Distillation, Packed column/
plate column distillation& Steam distillation and drying time in atmospheric and vacuum
dryer.
CO4: Determine the specific rate of dissolution & transfer coefficient for given solid and
mass transfer coefficient for air-water vapour system for various conditions using Wetted
wall column.

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 Department of Chemical Engineering MVJCE
CO5: Estimate the height of cooling tower for given situation & Verify vapour liquid
equilibrium.

Rules to be followed in laboratory

Do’s
A) Come well prepared for Lab Class.
B) Enter the lab with gloves & other protective apparel.
C) Try to know the physical & chemical properties of the chemicals that are used in the
experiments.
D) Handle the chemicals with at most care.
E) Replace the caps of the used chemical bottles.
F) Handle the electronic weighing balance carefully.
G) Clean the glassware before leaving the lab.
H) Switch off the power supply to all the equipment after completing the experiments.
I) Ensure proper flow of cold water to the condenser.
J) Regularly monitor the pressure of the boiler.
Don’ts
• Attend lab classes irregularly.
• Spill & mess the lab premises with chemicals.
• Handle the chemicals and equipments carelessly.
• Leave the broken glass pieces scattered in the lab.
• Leave the lab without informing the lab in-charge about the breakage.
• Waste power, chemicals, water etc.

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Sl. Page
Name of the Experiment
No. No.
01 Determination of diffusivity. 7-9
02 Verification of Rayleigh’s equation by conducting simple distillation. 10 - 12
03 Determination of HETP using packed column distillation. 14 - 17
04 Study the characterization of steam distillation. 18 -20
05 Solid-liquid leaching: single-stage and three-stage cross current. 21-24
06 Verification of Himus equation. 25-27
07 Study the drying characteristics in a tray dryer. 28-31
08 Adsorption Studies: single-stage and three stages cross current operation. 32-36
09 Determination of Vapour Liquid Equilibrium (VLE) data. 37-39
10 Liquid Extraction: single-stage and three stages cross current operation. 40-45
11 Hold up studies in packed columns. 46-47
12 Study the drying characteristics in a vacuum dryer. 48-50
Determination of mass transfer coefficient by conducting wetted wall
13 51-57
column experiment.
14 Measurement of cooling tower characteristic parameter. 58-61

15 Solid dissolution studies. 62-64

16 Separation of DNA using Gel- electrophoresis experiment. 65-67

17 The casting of the membrane. 68-70

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Experiment No.1 Date:

Determination of Diffusivity

Aim: To determine the diffusion coefficient (diffusivity) of organic vapor in the air.
Apparatus: Arnold Cell, magnetic Stirrer, heater, a beaker with hot water, Thermometer,
Stop-watch/clock, organic liquid.
Theory: Molecular diffusion is concerned with the movement of individual molecules
through a substance by virtue of its thermal energy. The phenomenon of molecular diffusion
ultimately leads to completely uniform concentration of substance throughout a solution,
which my, initially have been non-uniform. The rate at which a substance (solute) moves in a
solution at any point in any direction depends on the concentration gradient at that point and
in that direction. To express quantitatively, an approximate rate is needed. The rates are
described in terms of molar flux, moles/(area) (time). The area measured is normal to the
direction of diffusion. There are two types of fluxes, J and N type often used to describe the
molecular diffusion.
J is defined as flux of a constituent relative to the molar velocities of all other constituents
and N is defined as the flux of a constituent relative to a fixed point or location in space. For
example, consider a fish swimming in a stream of water. The fisherman is most interested in
the rate at which a fish swims against the flowing current towards the bait, a fixed position.
This is analogous to N while the J flux is analogous to the velocity of fish relative to the
velocity of upstream. If the diffusion is purely by molecular motion requiring large time, then
J may be given by the equation.
𝑑𝐶𝐴
𝐽𝐴 = −𝐷𝐴𝐵 ( )
𝑑𝑧
DAB is the diffusivity of diffusion co-efficient of constituent A in solution B. This equation is
known as Fick’s (first) law of diffusion which to analogous Newton’s law of viscosity
(momentum transfer) and Fourier law of conduction (heat transfer) Two types of situations
are, often encountered in mass transfer operations: 1) constituent A diffusing in stagnant non
diffusing constituent B eg: Gas absorption where a solute gas like say NH3 in liquid water
(solvent) with no diffusion of water vapour in to the stream gaseous mixture of Air- NH3 or
Humidification operation where water diffuses in to the air stream with no Air diffusion in to
the water stream. The second situation involves diffusion of both A&B in counter- current
direction (equimolal) ex: Distillation operation where say Benzene and Toluene diffuses
across the interface i.e. Benzene (A) diffuses from vapour phase to liquid phase while
Toluene (B) diffuses from liquid to vapour phase.

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Procedure:
• Fill the beaker with about three-fourth water, switch on the magnetic Stirrer and the heater.
Also put on the auxiliary heater to speed up.
• Fill the cell with the given organic liquid such that both the liquids, inside & outside the cell
is at same level, maintain a steady constant temperature.
• Note the level of organic liquid from a datum line. Choose the centerline of horizontal tube
as datum line. Let this be z1.
• Stopwatch is started simultaneously, and time required for the organic liquid level to drop by
2 mm is noted.
• Read this distance from datum line as z2. Repeat the experiment at different constant
temperatures.

Observations:
1. Organic liquid (component A): Acetone.
2. Total pressure, PT: 760 mmHg = Pa.
3. Vapour pressure of component A at 1, PA1= mmHg = Pa.
Find PA1 using Antoine equation.
𝐵
𝐿𝑜𝑔𝑃𝑠𝑎𝑡 = 𝐴 − ( )
(𝐶+𝑇)
Where,
T = oC
Psat = PA1, mmHg
A, B, C= ANTOINE constants can be found from Handbook.
4. Vapour pressure of component A at 2, PA2 = 0 mmHg = Pa.
5. Vapour pressure of component B at 1, PB1 = PT - PA1 = mmHg= Pa.
6. Vapour pressure of component B at 2, PB2 = PT - PA2 = mmHg= Pa.
ᵒ
7. Absolute Temperature, T = C.
8. Molecular weight of Component A =
9. Density of organic liquid, ρ = s.g. × density of water, kg/m3.
To find the density of organic liquid using Specific gravity bottle
i. Weight of empty specific gravity bottle, W1 =
ii. Weight of 25ml of water W2 =
iii. Weight of 25ml of organic liquid, W3 =
iv. Specific Gravity, s.g. = (𝑊3− 𝑊1) =
(𝑊2− 𝑊1)

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10. To find the diffusivity, formula used:
𝑅𝑇𝑃𝐵𝑀 𝜌𝑎𝑐𝑒𝑡𝑜𝑛𝑒 (𝑍2−𝑍2)
2 1
𝐷𝐴𝐵 = 2 𝜃 𝑀𝐴𝑃𝑇(𝑃𝐴1−𝑃𝐴2)

Where,
DAB = Diffusivity of acetone in air, m2 / sec.
R = Universal gas constant = 8.314 x 103 J/kg mole oK
PBM = log mean pressure of B, mmHg.
(𝑃𝑇−0)−(𝑃𝑇−𝑃𝐴1)
𝑃𝐵𝑀 = 𝑃𝑇
𝑙𝑛( )
𝑃𝑇−𝑃𝐴1

ρAcetone = Density of Acetone, Kg/m2.

Z=Head of the liquid column, m.
PT = Total pressure, mmHg.
PA = Partial pressure of acetone, mmHg
θ = time required for the decrease in level of the acetone by 2mm, sec.
MA = Molecular weight of acetone.
Tabular Column
Sl Temp. Z2 Final Time, θ PA1 PBM DAB
No ( C) Height (cm) (sec) (Pa) (Pa) (m2/s)
1
2
3

Result:
The average of Diffusion coefficient is--------------------- m2/sec

Inference:
Viva Questions
• State Fick’s law?
• What are the different driving forces for diffusion?
• What is the role of molecular diffusion in mass transfer?
• What are steady state & unsteady state diffusion?
• What is the effect of agitation on diffusion coefficient?
• What is Knudsen diffusion?
• What is the unit of diffusion Co-efficient and what are the analog terms in Heat and
momentum transfer operations?
• What are the different conditions under which diffusivity is determined? Give mass transfer
operation for each.

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Experiment No. 2 Date:
Verification of Rayleigh’s equation by conducting simple distillation
Aim: To study the principles of simple distillation and verify the results with respect to the
Rayleigh’s equations for Methanol – Water system.
Apparatus: Simple distillation setup - 1, Conical flask - 7. Pipette - 1, Specific gravity bottle.
Theory: Simple distillation, as the name implies, is a distillation without any reflux. In this
type of distillation, the mixture is subjected to separation by vaporization by heating at very
slow heating rate, so that a small differential quantity of liquid mixture is vaporized. The
vapour formed which is in equilibrium, is immediately removed and condensed. Rayleigh
derived a simple equation as follows.
𝐹 𝑋𝐹 𝑑𝑥
𝑙𝑛 ( 𝑊 ) = ∫ 𝑦∗ − 𝑥
𝑋𝑊

Where,
F = kg-moles of feed.
W = kg-moles moles of residue.
XF = mole fraction of high volatile component in feed.
XW = mole fraction of high volatile component in residue.
y and x are the equilibrium mole fraction of more volatile component in vapor and
liquid respectively.
Rayleigh’s equation holds good under the following assumptions:
• The composition of liquid is uniform.
• The process is carried out slowly, so that vapors leaving the still are in equilibrium
with the still.
• There is no entrainment of the liquid with the vapour.
• There is no condensation of vapor before it reaches the condenser.
Procedure:
• Mix known volumes of Water-Methanol and determine the density of the mixture, using
specific gravity bottle method.
• Determine the Densities of pure components and convert volume fractions into mole
fractions of component Methanol.
• To obtain calibration chart plot Density (on Y- axis) vs. mole fraction of Methanol (on X –
axis).
• 100ml each of methanol and water are taken in a round bottom flask.

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• It is fitted with a heating device, the charge is boiled slowly at a low temperature (at about
60% heating rate) and the vapors are withdrawn as rapidly as they form to a condenser,
where they are liquefied and the condensate is collected in the receiver.
• The distillation is allowed to proceed till 3/4th of the flak contents have been distilled.
• The volumes of residue and distillate, with their specific gravity are measured after cooling
them.
Observation & Calculation:

Weight of empty sp.gr. Bottle ,w1, = gm

Weight of sp.gr. Bottle + Water,w2, = gm
Weight of sp.gr. Bottle +Methanol,w3, = gm
Room temperature, = C
Density of Water at Room temp. ρw = kg/m3 (from Perry)
Density of Methanol, M = (w3 - w1,)/ (w2 - w1) * w = kg/m3
Weight of (i)th mixture, Wi = gm
Density of the (i)th mixture , .i = kg/m3
[(i)th is a mixture prepared for calibration chart, which may range from 5 to 10]

Table (for calibration chart)

Volume of Weight
Sl. Volume of Mole Density
Water Of mixture
No. Methanol (ml) Fraction of A (kg/m3)
(ml) (gm)
01 00 10 W3 – W1 ----- M
02 02 08
03 04 06
04 05 05
05 06 04
06 08 02
07 10 00 W2 – W1 w
Equilibrium Data:
x 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
y*
y*-x
1/(y*-x)
Refer Perry’s Chemical Engineer’s Handbook for equilibrium data.
Draw a graph of 1/(y* - x) Vs x.
Moles of feed, F =
Mole fraction of Methanol, XF =
Volume of Distillate = ml

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Density of Distillate, .D = kg/m3
Mole fraction of Distillate ,xD = (from Calibration chart)
Average mol.wt. of Distillate ,MD = xD* (Mol.wt)A+ (1- xD)* (Mol.wt)B
Moles of distillate, D , = (Vol.* .D)/ MD = kgmoles
Volume of Residue = ml
Density of Residue, W = kg/m3
Mole fraction of Residue, xW = (from calibration chart)
Moles of Residue, W = F- D = kgmoles
By Simpson 3/8 th Rule –
𝑋𝑑
𝑑𝑥
∫ =
𝑦∗ − 𝑥
𝑋𝑓

Verification of Raleigh’s Eq-

𝐹 𝑑𝑥
ln ( ) = ∫ ∗
𝑤 𝑦 −𝑥

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Relative volatility = {ln (F xf/ W xw)}/ {ln F (1-xf)/W (1-xw)} =

Results:
Average relative volatility Experimental= Theoretical=
Viva Questions

• What is an ideal mixture?

• What does Raoults’ law state and when it is used?
• What does Henry’s law state? For what type of system is Henry’s law used?
• What is relative volatility? What is the effect of this on separation by distillation?
• Why is Simple distillation called as simple? What is the other name for it?
• For good separation by distillation the value of relative volatility should be equal to 1. Say
true or false.

• What is minimum reflux ratio? How is it determined?

• Write all the assumptions of McCabe Theile method.
• What are the different types of plates used in a distillation column?
• What are different types of distillation?

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Experiment No.3 Date:

Determination of HETP using packed column distillation.

Aim: To study the distillation process in each packed bed and to calculate Height Equivalent
to Theoretical Plate by Mc Cabe Thiele method, Fenske’s equation, and Chilton Colburn
Analogy under total reflux conditions.

Apparatus: Conical flask, Measuring jar, Pipette, Thermometer, Beaker, Weight box,
Density Bottle.

Theory: Distillation is separation operation based on the relative volatility of the

components. A binary mixture can be separated in to as pure a product as possible, by
returning a portion of top vapor condensed as reflux and a portion of liquid vaporized at the
bottom. Usually, a partial re-boiler is used and a total condenser at the top is used. Reflux,
which is defined as L/D where L is moles of liquid condensate returned to the top of the
column and D is the Moles of Distillate product withdrawn. Two extreme situations are
possible, a minimum reflux ratio for which  number of theoretical plates (of a plate
Column) or infinite depth/height of packing (of a packed column) may be required for desired
separation. On the other hand, a total reflux i.e. all the Vapors condensed and returned, for
which the number of theoretical plates/Height of packing is minimum. For practical it is a
compromise between the two extreme cases, called optimum reflux ratio. A correlation
between a packed and plate column can be obtained and this is known as H.E.T.P. (Height
Equivalent to Theoretical Plate) McCabe and Thiele devised a method with simplifying
assumption that constant molal up-rise of vapors takes place from plate to plate and constant
overflow of liquid takes place from plate to plate in both rectifying and stripping section.
Fenske’s derived an analytical equation under total reflux condition. In McCabe –Thiele
method, at total reflux condition, the stripping and rectifying section merges and feed plate
becomes insignificant.
Procedure:
1. 200ml each of methanol and water is taken in a round bottom flask and this mixture is
distilled (heating rate of about 80%) till the temperatures read constant, and reflux is allowed
for half an hour.
2. The distillate and residue are cooled and collected, and their densities are measured using
calibration curve.
3. For plotting calibration curve solutions of different volumes are prepared in a conical flask,
their specific gravity is determined by weighing each sample, taking it in Pyknometer or
specific gravity bottle.
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4. The compositions are determined using calibration curve plotted for density against
composition or concentration of methanol.

Observation and calculations:

Data for density composition plot:
Molecular weight of CH3OH = M1=
Molecular weight of water = M2 =
Height of the packed bed =
Weight of empty Sp.gr.bottle W1 = gm
Weight of Sp.gr.bottle + water W2 = gm
Weight of Sp.gr.bottle + organic liquid W3 = gm
Weight of Sp.gr.bottle +organic liquid in the distillate W4 = gm
Weight of Sp.gr.bottle +organic liquid in the residue W5 = gm
Weight of distillate = gm
Weight of residue = gm
Volume of Residue =
Volume of Distillate=
Room temp. Tl = C
Volume of mixture =
Specific Gravity of Distillate =
Specific Gravity of Residue =
Wt of Mole Density
Vol. of Vol. of
mixture fraction of (kg/m3) R.I. Values
A (ml) B (ml)
(gm) (xa)
00 10

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02 08
04 06
05 05
06 04
08 02
10 00
RI Value of Distillate =
RI value of Residue =
Mole fraction of Distillate, XD = (from graph)
Mole fraction of residue, XB = (from graph)
PA (mmHg)
PB (mmHg)
X
Y
= PA/PB

Equilibrium data for CH3OH-H2O System (in mole fraction)

Generate values of “x” from 0 to 1.0 at the interval of 0.1
find αavg
Mc-Cabe Thiele Method
From the plot of x vs. y, number of stages is found.
Number of stages, Nm+1 =
HETP = Height of the column/ Nm

Fenske’s Equation,
Nm+1 = log (xD*(1—xW ) / (1 -- xD )*xW ) / log α avg
HETP = Height of the column/ Nm

Chilton Colburn Equation: -

HETP = Height of the column/ NT

Results: HETP calculated using

1. Mc Cabe Thiele method=

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2. Fenske’s equation=
3. Chilton Colburn Analogy=

Viva Questions
• What is rectification?
• What are the major components of a continuous rectification unit?
• What are flooding and weeping conditions in a rectification column?
• What are the different types of packing materials used in packed column?
• What is reflux, reflux ratio, minimum reflux ratio?
• State the basic assumption for using McCabe Thiele method to calculate the theoretical
stages required for rectification.
• What are HTU, NTU and HETP? Where are they used?
• What is the reflux effect on the number of transfer units and height of transfer units?
• Define bubble point and dew point.
• Define different tray efficiencies in distillation operation.
• What are ideal plates and actual plates?
• Give the various applications of Industrial Packing.

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Experiment No.4 Date:

Study the characterization of steam distillation.

Aim: To study the properties of steam distillation, report the vaporization and the thermal
efficiencies and compare the values of distillation temperature obtained theoretically and in
experiment.
Apparatus: Setup --- 1, Conical flask --- 7. Pipette --- 1, Specific gravity bottle – 2 nos,
Steam
Theory: - Steam distillation is used industrially to purify liquids, which are immiscible with
water, and to remove bad odors from oils. When water is added to a high boiling liquid
immiscible with it, the total pressure exerted by the mixture above the liquid surface will be
the sum of the vapor pressures of the pure components and therefore the boiling point of the
mixture will be less than that of water at the given temperature. Because of this, even high
boiling liquids are made to boil at low temperature and their decomposition is avoided.
The steam consumption for steam distillation process is normally high. To decrease the steam
consumption either super-heated steam is used, or distillation is carried out under low
pressure.
Often the impure organic liquids are purified and thus separated from the impurities by steam
distillation Examples of applications of steam distillation are in purifying the essential oils
and edible vegetable oils. In the former, the volatile essential oils are separated from non-
volatile impurities. These non-volatile impurities remain in the residue. While in the latter
case, i.e., steam distillation the coloring and odor causing volatile components, is distilled off,
leaving the product, oil, in the Residue.
For a steam distillation operation, the component to be distilled should exert its full vapor
pressure at the distillation temperature as partial pressure in the vapor phase. But in practice,
due to improper mixing of steam with liquid, the partial pressure exerted is less than its vapor
pressure hence term vaporization efficiency exists.
Procedure:
1. 200ml of Nitrobenzene is taken in a distillation flask and steam is passed through the NB.
The heating rate for steam generation is kept at around 180 watts using the rheostat.

2. The vapors are condensed; two immiscible layers of NB and water are formed in the
distillate and residue, which are separated in a separating funnel.

3. Volumes of 2 layers both in the distillate and the residue are noted.

4. Ambient temperature and distillation temperature are also noted.

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5. Specific gravity of the pure NB and water is measured using specific gravity bottle.

6. Readings are tabulated, and graphs are plotted, calculations are done.
Calculation steps:
Volume of organic liquid in the distillate. VOD = ml
Weight of Sp.gr.bottle W1 = gm
Weight of Sp.gr.bottle + water W2 = gm
Weight of Sp.gr.bottle +organic liquid in the distillate W3 = gm
Room temp. Tl C
Density of water at Room temp. (from Perry) w = gm/cm3
Density of organic liquid in the distillate, oD = (W3-W1)/W2-W1) * w =
Weight of Sp.gr.bottle +organic liquid in the residue W4 = gm
Density of organic liquid in residue, oR = (W4-W1)/W2-W1) * w = gm/cm3
Density of aqueous liquid in distillate = density of aqueous liquid in Residue = Density of
water at Room temp. (from Perry), aD = aR = w

Mass of organic liquid in distillate, moD = VOD * aD = gm

Volume of aqueous layer in the distillate,VaD = ml
Mass of aqueous layer in the distillate, maD; VaD*w = gm
Moles of organic liquid in distillate, nA;; moD/ MA = gm moles
Moles of aqueous liquid in distillate, nB;; maD/ MB = gm moles
Actual mole ratio. N act = nA/ nB =
Theoretical mole ratio, Nth = PA/ PT-PA (from Fig.3) =
Vaporization Efficiency = N act / Nth x 100 =
Volume of organic liquid in the residue VOR = ml
Volume of aqueous layer in the residue ,VaR = ml
Mass of organic liquid in residue moR = VOR * aD = gm
Mass of aqueous layer in theresidue, maR; VaD*w =gm
Thermal Efficiency, = A/B
Where A is theoritical steam required/ gm. of organic liquid
A = {[ (R+1) CP(Td-Tl) + OL / W + (100-Td)] +[ (PB/PA)* (MB/MA)]}
Where ‘R’is the ratio of mass organic liquid in residue, mOR, to that of in distillate, moD
mOR,/moD ;
OL is latent heat of organic liquid and this is obtained as
OL = W [ln (PB/PA) ] * (MB/MA) where ln (PB/PA) is the slope of Othmer’s plot

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Td is the distillation temperature; Tl is room temperature

B, Actual steam consumption,

(Mass of aqueous phase in distillate + mass of aqueous phase in residue)

(Mass of organic liquid in distillate )

Thermal Efficiency = A/B

Note: - Suffix A, o, OL etc refers to organic liquid /layer/phase and

Suffix B, a, W etc refers to aqueous (water) liquid/ layer/phase
MA refers to molecular weight of organic liquid
MB refers to molecular weight of aqueous liquid (Water) = 18.

Result:-
Distillation Temperature (Expt) = C
Distillation Temperature (Th, from Fig.3) = C
Vaporization Efficiency =
Thermal Efficiency =

Viva Questions

1. For good separation by distillation the value of relative volatility should be equal to 1.
Say true or false.
2. For a mixture of two components A & B with AB<1. Which component is more volatile?
3. What is the primary requirement of a liquid subjected to steam distillation?
4. What are the characteristics of steam distillation?
5. What are different types of steam distillation based on the condition of steam?

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Experiment No.5 Date:

Solid-Liquid Leaching: Single stage and three stage cross current

Aim: To study the principles of cross current leaching and compare the results obtained for
leaching of a mixture of oxalic acid and sand, by
a) 3- stage process
b) single – stage process

Apparatus: Stoppered Conical Flask 250 ml –4; Burette 50 ml –1; pipette 10 ml-2 Conical
flasks 100ml –3; Measuring Jar 100 ml –1, volumetric flasks 250ml - 4,100 ml-1.
Chemicals: De-Ionized water; (B-solvent) sand (A inert) Oxalic Acid (C solute), 0.1 N
NaOH

Theory: Leaching is a process of recovering a solute from a solid using a solvent. Two steps
are involved in leaching.
1. Contact of solid and solvent to effect transfer of solute to the solvent.
2. Separation of the resulting solution from the inert solid.
Leaching may be carried out by any one of the ways.
a) Single stage
b) Multi stage crosscurrent
c) Multi stage counter current
In a single stage operation, the feed and fresh solvent are contacted in a conical flask and
mixed for a sufficient time for the solute to be transferred to the liquid phase. The solution
and the solids are separated as overflow and underflow respectively.
In a multistage cross current system, the feed and fresh solvent are contacted in a conical
flask and mixed in the first stage. The underflow from the first stage is sent to the second
stage where some fresh solvent is added. The same procedure is repeated successively.
The Water –sand-Oxalic Acid constitutes a system of ‘constant under-flow’
The solute solid distributes in equal proportions with water (solvent) and solid associated
with inert solid, sand. The equilibrium relationship then simplifies as a straight line of 45
line. The distribution coefficient, m = y*/x = 1

Procedure:
Standardization of solutions:

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• Prepare 0.1 N oxalic acid by weighing 0.63 gm of the salt and making up to 100ml in a
volumetric flask.
• Titrate std. oxalic acid solution against NaOH solution and determine its normality.
Single Stage operation:
1. Take 100 gm of wet sand in to a 250 ml conical flask add 2 gm of oxalic acid crystals.
2. Mix well and add 150 ml of water.
3. Shake thoroughly for 30 min and allow the solids to settle.
4. Carefully, decant the clear liquid (supernatant) to a 250 ml standard (volumetric) flask
and make it up to the mark.
5. Take portions of 10 ml sample and titrate against NaOH solution to get concordant
values.
Three stage cross current operation:
• To 100 gm of wet sand in a 250 ml conical flask add 2 gm of oxalic acid mix well and add
50 ml water (solvent).
• Shake thoroughly for 10 min. Allow to settle and decant supernatant liquid to a 250 ml
volumetric flask, make up to the mark.
• Titrate 10ml sample against NaOH solution to get concordant values to the residual sand-OA
mixture add another 50 ml water, shake for 10 min. settle, decant.
• Titrate make-up samples against NaOH solution to get concordant values.
• Repeat the whole procedure of adding 50 ml of water to titration to constitute the third cross
current stage.

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Observations & Calculations:
Normality of Oxalic Acid = 0.1 N
Normality of NaOH solution = N

Volume of Volume of over Volume of

Normality of
Stages water taken flow taken out NaOH run
oxalic acid
(ml) (ml) down (ml)
Single
Multistage I
II
III

Single Stage Operation: Calculations

Volume of NaOH added (concordant value) =
Normality of sample, Nsample =(VNaOH x NNaOH) /(Vsample =10) =
Initial quantity of solute (OA) taken = 2gm
Quantity of OA leached = ( Nsamplex 63*volume of water added(150ml)) /1000 , = w
% OA leached (Expt) = (w/2) x 100
% OA leached (Graphical) & Stage  calculations are identical to that explained for Liq-Liq
Extraction excepting for the fact that the equilibrium is simply the Diagonal for leaching
operations
Three Stage Cross Current Operations: Calculations
Follow the calculations of Single stage for Stage1, Stage2 & Stage3 and evaluate w1 ,w2 &w3
% OA leached (Expt) = [ (w1 +w2 +w3)/2] x 100
Similarly calculate for each of three stages and compute total OA leached And compare
the % increase of OA leached in a 3 stages cross current over that of a single stage.
% increase of leached= (ao–a)/(ao)*100

Result:
Single Stage (a) Three Stage % Increase of
Cross Current (a0) OA leached
Experimental

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Viva Questions
• What is cross-current, co-current and counter-current operation in leaching, extraction, and
adsorption operation?
• What is the equilibrium line for leaching operations?
• What is meant by constant under flow condition and what is the analogous term in
distillation?
• Give some examples of solid liquid leaching
• Mention the sample, solute, solvent, and type of operation in the above experiment.
• What are the examples of solid liquid operations in mass transfer operations?
• What does the x and y represent in the equilibrium curve of solid liquid leaching?
• What is cross-current, co-current and counter-current operation in leaching operations?
• Explain the principles of extraction and leaching. Give industrial applications of these
operations.
• List out the equipment’s for leaching operations.

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Experiment No.6 Date:

Verification of Himus equation

Aim: To verify the law of surface evaporation and to obtain constants of Himus equation.

Apparatus: Set up, thermometer and stopwatch.

Theory: When a liquid surface is kept open to atmosphere a concentration gradient is set in
between the liquid surface and the atmospheric air. At the liquid surface the partial pressure
of the liquid vapour will be the vapour pressure of the liquid at the surface temperature. The
partial pressure of the liquid vapour far away from the liquid surface is determined by the
amount of liquid vapour present (humidity) in the atmosphere. Because of this concentration
difference there will be a steady transfer of liquid vapour into the atmosphere, or the liquid
will evaporate.
The steady rate of evaporation of water is given by the Himus equation:
dW
( )
n
= k Pi - Pg
Ad
where:
dW = mass of water evaporated, = kg
A = Area of evaporating surface, = m2
dθ = time taken for evaporating dW kg water, = hrs.
Pi = vapour pressure of water at surface temperature, = mm Hg
Pg = partial pressure of water in air, = mm Hg
k and n are Himus constants
The values of the constants k and n are calculated by conducting different sets of evaporation
experiments at different temperatures.
Procedure:
• Fill the beaker to about three-fourth and note down the temperature and initial weight of the
water.
• Note down the time taken for reducing 2 gm of the initial weight.
• Repeat the above procedure at other constant temperatures (say 50C; 60C up to 90C).
• Note the dry & wet bulb temperatures.
• Measure the inside diameter of the beaker.
• From ‘Perry’s Handbook read the vapour pressures of water at these temperatures such as
40C, 50C; 60C up to 90C.

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Observation & Data (Specifications):

Diameter of the beaker : 10 × 10-2(m)

Area : (m2)
Dry bulb temperature : (C)
Wet bulb temperature : (C)
Humidity (from Psychrometric chart) : H (kg water/kg dry air.)
Partial Pressure of water vapour, P : [H *(29/18) PT]
(Where H is Humidity, 29 and 18 molecular
: (mm Hg)
weights of air and water respectively)
PT, total (atmospheric) pressure : 760 mm Hg

Vapor Time w
Wt. of water log( ) log( P* − P)
Sl. Temp Pressure, requi W 
No P*
Evaporated,
red A( )
( C) (gm) (Sec)
W (gm)
(mm Hg)  (Sec)
1 2
2 2
3 2
4 2
5 2

Result: Himus Equation Constants n (slope) =

k (intercept) =

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Viva Questions
1. What is the use of Himus Equation?
2. Can you predict the loss of water per day from a pond from the result of experiment on
surface evaporation? What is the underlying basic assumption?
3. When the partial pressure of the vapor in contact with the liquid equals the vapour
pressure of the liquid, the rate of evaporation is zero. State whether the statement is true
or false. Justify your answer.
4. What are saturation pressure and temperature?
5. What is the driving force for surface evaporation?
6. Does the rate of surface evaporation depend on the humidity of air?
7. What is wet bulb temperature?
8. Does the wet bulb temperature be greater than or lesser than dry bulb temperature?
9. What is adiabatic saturation temperature?
10. Theoretically when should the evaporation from the surface of a liquid stop?
11. What is percentage saturation and relative saturation?
12. Can you determine the diffusivity of water at different temperatures using your surface
evaporation set up? If yes How?

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Experiment No.7 Date:

Study the drying characteristics in a tray dryer

Aim: To draw the rate of drying curve for air-drying of the given sample at constant drying
conditions and to find
1. The critical moisture content and
2. Equilibrium moisture content.

Apparatus: Tray Dryer set up, stopwatch/clock, wet and dry bulb thermometers.

Theory: Drying is a simultaneous heat & mass transfer operation involving the removal of
moisture from wet solid by contacting with hot air. The air in turn gets humidified, if the
solid is kept in a chamber over a tray and air is passed over the plate/tray the dryer Is
generally known as atmospheric tray dryer. However more common type is Rotary dryer
where wet solid and hot air move through the inclined rotary dryer counter-currently,
moisture from wet solid lost to hot air. During drying, there are, generally, two stages of
drying constant rate and falling rate. In the constant rate period, drying proceeds by diffusion
of vapour from the saturated surface of the solid across the air film. Moisture movement
within the solid is rapid enough to maintain a saturated condition at the surface and the rate of
drying is controlled by the rate of heat transfer rate to the evaporating surface. The mass
transfer rate balances the heat transfer rate temp. Humidity, velocity and direction of flow all
remain constant and hence the name constant rate period. Once sufficient moisture is
removed, the rate continuously falls and this stage is called as falling rate period. In some
types of solids there are two falling rate period, first a linear rate followed by a nonlinear
period.
Following are a few important definitions in drying operations

Moisture content, wet basis: (kg moisture / (kg dry solid + kg moisture) x 100. If ‘X’ is the
kg moisture / kg dry solid. Then the Moisture content, wet basis is X/ (1+X) Percent Moisture
content, wet basis is then 100X/ (1+X)

Moisture content, dry basis: X and Percent Moisture content, dry basis is then 100X

Equilibrium moisture content, X*: this is defined as the moisture content of a substance is
in equilibrium with partial pressure of air. Further removal of moisture beyond this is not
possible without changing the conditions of the air.

Bound Moisture: This refers to the moisture contained by a substance, which exerts an
equilibrium vapor pressure, which is less than that of the pure liquid at same temperature.

Unbound Moisture: This refers to the moisture contained by a substance which exerts an
equilibrium vapor pressure which is equal to that of the pure liquid at same temperature.

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Free Moisture: This is the moisture contained by a substance in excess of equilibrium
Moisture, X- X*. Only free moisture can be removed by evaporation. This moisture content
of a solid depends on the vapor concentration in the gas.

Figure 1: Drying Curve

Xc is called as critical moisture content, which signifies the end of constant rate period and
beginning of falling period (first).
Procedure:
1. The pan in the batch drier is initially weighed
2. Then 100gm of sand is taken in it.
3. Now the sand is wetted with water using a pipette so that entire mass is wetted and is
spread uniformly over the pan.
4. The pan along with the wet sand is placed in the drier and balance is adjusted to read
zero and the pan is taken out.
5. 2 thermometers are placed in position to read dry and wet bulb temperatures.
6. When the incoming hot air reads a temperature of 80ºC, the pan is introduced in the
setup.
7. The drier door is closed and a weight of 2 gm is removed from the balance.
8. Simultaneously stop watch is started.
9. Time taken for the balance to read zero again is noted down.
10. The procedure is repeated till all the moisture content is removed completely by
measuring time continuously.
11. Readings are tabulated, calculations done and graphs plotted.
12. Repeat whole experiment with another sample say, calcium carbonate.

Observation & Data

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Diameter of tray, D = 16.5cm
Drying Area, A =  D 2/4 = [ m2 ]
Drying rate, N = ∆w /A∆t where Δw = change in weight, = 2 gm or 2x 10-3 kg
Weight of dry solid w1= gm or w1x 10-3 kg.
Weight .of Pan =
Weight .of Pan +sand =
Weight .of Pan +wetted sand =
S.No Time Weight ∆w ∆t N= ∆w /A∆t 1/N Moisture content(X)
(min) (gms) (g) (min) (kg/m2s) (kg of moisture/kg of dry solid)
5
5
5
5

Plot graph N vs X and 1/N vs X

Theoretical time of drying for removal of moisture from X1 to X2

ttotal = tc + tf where tc is time of constant rate period and tf is time of falling rate period

W (X1-Xc)
Time of constant rate period, tc = -----------
AN*

W
Time of falling rate period, tf = --- * area under the
A curve of Fig. 3

Result: Critical moisture content (from Fig.2) =

Equilibrium moisture content (from Fig.2) =
Total time of drying =

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Viva Questions
1. What are drying characteristics?
2. What are bound and unbound moisture?
3. Saturated air will be used for drying wet material. True or false.
4. The maximum temperature attained by air during drying will be (a) equal to dry bulb
temperature (b) greater than dry bulb temperature (c) equal to wet bulb temperature (d)
greater than wet bulb temperature.
5. What is critical and equilibrium moisture content.
6. Explain the drying mechanism for different rate periods.
7. For identical condition of (inlet air, initial moisture content, Weight of dry solid, Surface
area). In which of the two i.e., atmospheric tray dryer and vacuum dryer you expect
faster rate of drying. Justify.
8. The moisture content of the dried material is (a) less than the critical moisture content
(b) equal to the critical moisture content (c) greater than the critical moisture content.

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Experiment No.8 Date:

Adsorption studies: Single stage and two stage cross current operation
Aim: To determine the constants of Freundlich Equation from given data and determine
increase in percentage of adsorption in a two stage cross current operation over a single
stage operation both experimentally and theoretically.

Apparatus: Flask shaker, conical flasks, filter papers, burettes, pipettes, Oxalic Acid
Activated Carbon /Charcoal, NaOH, phenolphthalein indicator solution.

Theory: Adsorption is a mass transfer operation used to separate the desired constituents in a
fluid mixture by contacting with certain solid where the constituent gets attached (adsorbed)
on the solid surface. To recover the constituent has to be desorbed. A similar operation with
an exception that the direction of transfer is reversed. There are two types of adsorption
operations. (i) a physical phenomena where the constituent is recovered in the same form as it
were present in the fluid mixture. The force of attraction by which the constituent is attached
with solid surface is vanderwaal (weak) type only.
(ii) A chemisorption where a the constituent under goes chemical reaction and on desorption
the product of chemical reaction between the constituent and solid material but not the
constituent. Examples of physical adsorption are removal of colouring matter from sugar
syrup, removal of colouring matter & odour causing constituents from vegetable oils
(refining of vegetable oils) while that of chemisorption are heterogeneous non-catalytic
reaction (burning of coal) and a majority of solid catalytic reactions. Thin film coating for
electronics device manufacturing etc. chemisorption is a separate topic of reaction
engineering. The fluid mixture may be a gas mixture or a liquid mixture. All solids are not
capable of effecting the separation. Only a few solid substances are capable of adsorbing a a
particular constituent. Further these solids are to be specially prepared as activated carbon
Following a list of a few adsorbents (solids) and adsorbates (constituents adsorbed) Fuller’s
Earth : natural clays, (Megnesium and Calcium silicates) used for decolorizing, neutralizing
and drying of petroleum products like lubricating & transformer oils, kerosine and Gasoline
(other adsorbents for above constituents are Activated Clays, Bauxite) Bone Char : Used for
refining sugar (other adsorbents are Activated charcoal , Activated carbon )
Alumina: hard, hydrated Aluminum Oxide used chiefly as desiccant for gases and liquids
Activated Carbon: this is most widely used adsorbent prepared from coconut shells, fruit pits,
coal etc and used for variety of purposes like decolorizing of sugar solutions, industrial
chemicals, drugs, water purification, refining of vegetable oils, recovery of Gold & Silver
from cyanide ore-leach solution.

Molecular Sieves: These are porous synthetic zeolites metal Aluminosilicates . They are
used for separation of gas and liquid hydrocarbon mixtures, dehydration of gases and liquids.

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Silica Gel: These are prepared as gels by acid treatment of sodium silicate solution These are
principally used as desiccants and thin layer chromatography.

Adsorption Equilibrium (Adsorption Isotherms)

Adsorption of Liquids: heat of wetting is the evolution of heat when an adsorbent is
immersed in a liquid /solution. When an adsorbent is a say, binary solution, both solute and
solvent are adsorbed. As total adsorption cannot be measured only preferential adsorption of
solute is often measured. The usual practice is to treat a known volume of solution with
known weight of adsorbent,  vol. solution/mass adsorbent. As a result of preferential
adsorption of the solute, the concentration of the solute fall from Co to C* (where C* is the
equilibrium concentration) then the quantity of solute adsorbed is, neglecting the volume
changes, is ( Co-C*) , mass solute adsorbed/mass adsorbent. Unit of Co & C* is then mass
of solute/ volume of solvents. Freundlich Equation over small concentration range,
particularly for dilute solution, the Adsorption is described by an empirical equation called
Freundlich Equation as
C* = k [( Co-C*)] n

Adsorption operations: Single stage and multistage cross current operations

Fig. 1 Single Stage Fig. 2 Multi Stage Cross Current

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Procedure:
(i) Preparation and standardization of solutions:
1. Prepare 0.1 N oxalic acid. Prepare 0.1N NaOH solution (approximately) Standardize the
NaOH solution.
Single Stage operation:
1. Take 75 ml of 0.1N oxalic acid in a 250 ml stoppered conical flask add 2.0 gm of
activated carbon to it.
2. Clamp the flask in a flask shaker and shake for 30 min.
3. stop after shaking, filter and titrate the filtrate with standard NaOH solution.
4. Titrate for concordant values.
Two Stage cross current operation:
1. Take 75 ml of 0.1N oxalic acid in a 250 ml stoppered conical flask add 1.0 gm of
activated carbon to it.
2. Clamp the flask in a flask shaker and shake for 15 min.
3. stop after shaking, filter and add to the filtrate another 1.0 gm of activated carbon and
shake for additional 15 min. (total 30 min).
4. Again, filtrate and titrate the filtrate with standard NaOH solution. Titrate for
concordant values.
Observation, Data & Calculation

Equilibrium data of Freundlich equation C* =k [(CO - C*)] n

X, (CO - 0.332 0.2 0.153 0.132 0.114 0.102

C*)
Y*103, C* 04.08 3.621 3.225 2.772 2.459 2.217
2

Fig. 3:
Normality of Oxalic Acid = 0.1 gm eq/lit (N1)
Normality of NaOH solution = N2
Initial concentration of Oxalic acid, CO = 0.0063 gm OA (solute) /gm water (solvent)
SINGLE STAGE: CALULATION:
Volume of NaOH added (concordent titre value) = a ml

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Y = ( a x N2 x63 )/ (10x 1000 ) = ‘m’ gm OA /gm water
% OA adsorbed (Expt) = (0.0063-m) /0.0063 x 100
% OA adsorbed (graphical) =

Draw the equilibrium line Y*103 vs X (fig .4) from given data
Draw the operating line with a slope of – Ss/Ls where Ss is the weight of adsorbent
(Activated Carbon) and Ls is the weight of 0.1N OA (solvent)
Read from graph Yss then % OA leached (graphical) = (0.0063- Yss) /0.0063 x 100
[ss is single stage]
% OA adsorbed (from Freundlich constants)
Calculate Y1 from Freundlich Equation by substituting the k and n values from Fig 3
Ss /Ls = (Yo –Y1 ) / (Yo /k)1/n where Ss & Ls are quantities of Activated carbon & oxalicAcid
Solutions, Yo is the initial concentration of OA = Co

TWO STAGE CROSS CURRENT: CALCULATIONS

Volume of NaOH added to first stage (concordant titre value) = b1 ml
Y1= (b1xN2x63)/(10x1000) = p1 gm OA /gm water
Volume of NaOH added to second stage (concordant titre value = b2 ml
Y2 = (b2xN2x63)/(10x1000) = p2 gm OA /gm water
% OA adsorbed (Expt) = (0.0063- p2) /0.0063 x 100
% OA adsorbed (graphical) =
Draw the equilibrium line Y* vs X (fig .4) from given data
Draw the operating line with a slope of – Ss1 /Ls1 where Ss1 is the weight of adsorbent
(activated Carbon) and Ls1 is the weight of 0.1N OA (solvent)
Read from graph Y1 then % OA leached (graphical) = (0.0063- Yss) /0.0063 * 100
Then from Y1 draw the operating line for second stage as – Ss2 /Ls2 and read Y2
% OA adsorbed (graphical) = (0.0063-Y 2)/0.0063 x100
% OA adsorbed from Freundlich constants)
Calculate Y1 &Y2 from Freundlich Equation from Ss1 /Ls = (Yo –Y1 ) / (Yo /k)1/n &
Ss2 /Ls = (Y1–Y2) / (Y1 /k)1/n where Ss1 , S s1 & Ls are quantities of Activated carbon & oxalic
solutions, Yo is the initial concentration of OA = Co
% Increase of OA adsorbed = (ao–a)/(ao)*100

Result:

Single Two Stage % Increase of

Stage (a) Cross Current (a0) OA adsorbed
Experimental
Graphical

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Viva Questions

1. What is Freundlich adsorption isotherm and why in adsorption alone the word isotherm is
specially used.
2. Define differential and integral heats of adsorption.
3. Name a few adsorbents and their applications.
4. What are molecular sieves?
5. What are the different types of adsorptions? Give industrial applications for each type.
6. What is enhancement factor?
7. What modification in mass transfer theories is involved when mass transfer is
accompanied by chemical reaction?
8. Different adsorbents are used for different systems. True or false.
9. What is deactivation of adsorbent?
10. What is regeneration of adsorbents?
11. What type of diffusion occurs in adsorption?

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Experiment No.9 Date:

Determination of vapor-liquid equilibrium (VLE)

Aim: To determine VLE data using a device that ensures equilibrium between the liquid and
the vapor.
Theory: Equilibrium is a static condition in which no changes occur in the macroscopic
properties of a system with time. Vapor-liquid equilibrium is a condition where a liquid and
its vapor are in equilibrium with each other, a condition or state where the rate of evaporation
is equal to the rate of condensation one a molecular level such that there is no overall vapor-
liquid inter-conversion.
In theory equilibrium takes forever to reach, such equilibrium is practically reached in a
relatively closed location if a liquid and its vapor are allowed to stand in contact with each
other long enough with no interference or only gradual interference from the outside.
Relative volatility (a) is a measure comparing the vapor pressures of the components in a
liquid mixture. When the volatilities of both key components are equal, a = 1 and separation
would be impossible under the given conditions because the compositions of the liquid and
the vapor phase are the same (azeotropic).As the value of a increases above 1, separation
becomes progressively easier.

VLE Experimental Setup :

2. The setup consists of a round bottom flask, a condenser, a thermocouple, two water
streams a heater and a conical flask.
3. A mixture of methanol and toluene is prepared and put into the flask. Then the power is
supplied and the mixture begins to boil.
4. After some time equilibrium is reached, this is marked by steady temperature in both the
phases.
5. Samples of condensed vapor and liquid are taken. To calculate the composition we need
to measure the refractive index of the sample.
In an experiment since vapor and liquid composition changes dynamically we need to
measure until they reach vapor liquid equilibrium. For such a measurement, physical
properties (such as refractive index) can be explored and related to the composition of a

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liquid. Now we first prepare a calibration chart that depicts the variation of refractive index
with composition

Procedure:

1. Cleaning the Setup: The setup is cleaned to start a new Experiment.

2. Mixing in given ratios: A mixture of benzene and toluene is prepared and put into the
flask.
3. Power is supplied: Then the power is supplied, and the mixture begins to boil.
4. Equilibrium is reached: After some time equilibrium is reached, this is marked by steady
temperature in both the phases.
5. Measuring RI: Samples of condensed vapor and liquid are taken. To calculate the
composition, we need to measure the refractive index of the sample and look into the
chart.
6. Plot the VLE data.
Observations & Calculations:
Tabular Column:
S NO Time (min) Temperature RI x y
(◦C) x y

VLE
(1 atm)
Temp ( C )

0 0.2 0.4 0.6 0.8 1

Mole Fraction (Lower Boiling Point)

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Result:
Viva Questions

1. What is relative volatility?

2. To separate a binary mixture relative volatility should be?
3. VLE data once obtained is represented on which scale?
4. The Relative Volatility of components i and j can be defined as?
5. Given that αAB=2.0, Then equilibrium ratio of B is KB=0.7, Estimate αBA ?

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Experiment No: 10 Date:

Liquid extraction: Single and three-stage cross current operation

Aim: To carry out Extraction in three-stage cross current operations and in single Stage
operations and find the % increase in solute extracted by three-stage cross current.
Apparatus: Flask Shaker-1, Stoppered Conical Flask (250 ml) –4, Separating Funnel (250
ml) –2, measuring jars (100 ml) –2, Specific Gravity Bottles (10 ml) –2, test tubes –5, Abbe-
Refractometer.

Chemicals: De-Ionized water (B-solvent) Benzene (A-Diluent) and Isopropyl Alcohol (IPA)
(C-solute)

Theory: The extraction of a compound form one phase to another is based on solubility
differences of the compound in one phase relative to other. When a compound is distributed
between two immiscible liquids, the ratio of the concentrations in two phases is known as
distribution coefficient:

KD = Yl/XH, where Yl and XH are concentrations of solute in light and heavy phases
respectively.

The Water –Benzene and IPA constitutes a system of ‘Immiscible liquids’ i.e. water and
Benzene are insoluble in each other for all concentrations. For such a system if solvent (B) is
added to a binary homogeneous liquid mixture (A-C) containing a diluent (A) and a solute
(C) , then C separates (distributes it self) between A and B with no mixing of A and B. Such
mixing and then separating two heterogeneous liquids constitutes a Stage and if the exit
streams are in equilibrium, then a combination of mixing and separating operations is known
as an equilibrium stage. The two liquid phases are accordingly called as ‘Extract’ (solvent
rich phase) and ‘Raffinate’ (diluent rich phase). If the operations are carried out in a such a
manner that if the fresh solvent is added to ‘raffinate phase’ then the operation is termed as
cross-current operations.
Liquid extraction is commonly used to separate inhibitory fermentation products such as
ethanol and acetone- Butanol from a fermentation broth. Antibiotics are also recovered by
liquid extraction (amylacetate and isoamylacetate). Ideally, the liquid extractant should be
nontoxic, selective, inexpensive and immiscible with fermentation broth and should have a
high distribution coefficient for the product.

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Fig. 1 Single Stage Fig. 2 Multi Stage Cross Current

X
For insoluble liquid system, the equilibrium concentrations are plotted as X = &
1− X
Y
Y = . Since the liquids are insoluble, there are A kg of the substances in all raffinates.
1− Y
Similarly, the extract from each stage contains all solvent B fed to that stage Solute balance
about any stage, n, is then
Axn−1 + Bys = Bnyn + Axn → (1)
A ys − yn
= → (2)
Bn xn−1 − xn

Procedure:
Preparation of Calibration chart of (1) Benzene-IPA
Prepare mixtures of 5:0,1:4, 2:3, 2.5:2.5, 3:2,4:1 and 0:5 volume proportions of Benzene and
IPA (total volume 5ml) and Read their Refractive Indices (RI values) in an Abbe
Refractometer. Also read RI values of pure Benzene and IPA. Convert the volume ratios into
mass fraction of IPA in Benzene and plot RI (y axis) vs. Mass fractions (x axis). Similarly
prepare mixtures of 5:0,1:4,2:3, 2.5:2.5, 3:2,4:1 and 0:5 volume proportions of water and IPA
(total volume 10 ml) and determine their density. Also determine the density of pure IPA.
Take the density data of water at room temp from Perry’s Hand Book. Convert the volume
ratios in to mass fractions of IPA in water. Plot density (y axis) vs. mass fraction (x axis).

Single Stage operation:

To 80 ml of Benzene mix 5ml IPA and to this mixture add 120 ml water (solvent) in a conical
flask. Stopper the flask and keep it in the flask shaker and shake for 30 minutes, after 30
minutes, remove the flask and separate the two layers using separating funnel. Take a sample
of organic phase and read its RI. And from calibration chart of RI vs. Mass fraction find the
composition of IPA in raffinate, x. Like wise find composition of IPA in extract, y. (from
calibration chart of Density vs mass fraction)

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Three stage cross current operation: To 80 ml of Benzene mix 5ml IPA and to this mixture
add 40 ml water (solvent) in a conical flask. Stopper the flask and keep it in the flask shaker
and shake for 10 min. Remove the flask, separate the two layer and to the organic layer add
another 40 ml and shake for 10 min. after this 25 min repeat by adding yet another volume of
40 ml of water and shaking for next 10 min. (total water added =120 ml and total time =30
min)

[The experiment can be started simultaneously by adding required quantities into 4 flasks,
shaking one flask for 30 min continuously while removing the other 3 flasks after 10 min.
Calibration chart can be prepared while the flasks are kept for shaking]
Observation &Calculations:
Room Temperature (TR ) = C
Density of water at TR , A (from perry) = gm/cm3
Weight of empty sp.gr. bottle , w1 = gm
Weight of sp.gr. bottle + water w2 = gm
Weight of sp.gr. bottle + IPA w3 = gm
Weight of sp.gr. bottle + Benzene w4 = gm
Density of IPA, c = [ (w3 - w1) / (w2 - w1)]* A = gm/cm3
Density of Benzene, B = [(w4 - w1) / (w2 - w1)]* A = gm/cm3
Tabular Column for IPA- Benzene
SL No Vol of IPA Vol of Benzene Mass Fraction of R.I
IPA
1 0 5
2 1 4
3 2 3
4 3 2
5 4 1
6 5 0
Tabular Column for IPA- Water
SL No Vol of IPA Vol of Water Mass Fraction of R.I
IPA
1 0 5
2 1 4
3 2 3
4 3 2
5 4 1
6 5 0
Equilibrium Data:
X 0 0.023 0.031 0.039 0.047 0.061 0.073
Y 0 0.053 0.075 0.081 0.087 0.111 0.136

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Single Stage Operation Calculations:
R.I of Organic Layer (Raffinate Layer) =
Mass Fraction of IPA in Raffinate (from Calibration graph), xR =
xR
Mass ratio of IPA in Raffinate, xR=
1− xR

5ml  c mc
Mass ratio IPA in Benzene feed, xF = = , where m C & m A are mass of IPA
80  A mA
and Benzene in feed, respectively.
Mass of IPA extracted = (xF - xR )  m A = gm
x − xR
% IPA extracted = F 100 (experimental)
xF
To calculate % IPA extracted (graphically, theoretically)
Draw the equilibrium (distribution) curve, (y*vs. x)

Locate x F on x-axis. Draw a line with a slope of - m / m

A B =(-A/B), to cut the equilibrium
curve, read on y-axis as y*E and x coordinate as x R,Then % IPA extracted

x − xR
= F 100
xF
y'*E − yE
Stage  of single stage = 100
xR − xF
Where yE and x”R are experimental values.

Three Stage Operation Calculations:

Stage1:
R.I of Organic Layer (Raffinate Layer) =
Mass Fraction of IPA in Raffinate (from Caliberation Chart), xR1 =

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xR
Mass ratio of IPA in Raffinate, xR1′= 1

1 − x R1
Mass of IPA extracted , m1= (xF′ - xR1 )  m A
′
= gm

Stage2:1
R.I of Organic Layer (Raffinate Layer) =
Mass Fraction of IPA in Raffinate (from Caliberation Graph), xR2 =

x R2
Mass ratio of IPA in Raffinate, xR2′=
1− x R 2
Mass of IPA extracted , m2= (xF - xR2 )  m A = gm
′ ′

Stage3:
R.I of Organic Layer (Raffinate Layer) =
Mass Fraction of IPA in Raffinate (from Calibration Chart), xR3 =

x R3
Mass ratio of IPA in Raffinate, xR3′=
1− xR3
Mass of IPA extracted , m3= (xF′ - xR3′ )  m A = gm

Total mass of IPA extracted, m = m1+m2+m3

m
% IPA extracted =
x 
F

Similarly calculate for each of three stages and compute total IPA extracted & compare the %
increase of IPA extracted in a 3 stages cross current over that of a single stage. Also calculate
stage  for 1st, 2nd and 3rd stage of the 3 stages cross –current operation. (See the graph)

For a given number of cross current stages, feed quantity & composition, solvent quantity and
composition (usually zero), the raffinate concentration, quantity and composition, extract
quantity can be determined, using equation (2). This is called operating line or material
balance equation
% Increase of IPA Extracted=(ao–a)/(ao)*100

Result:

Single Three Stage % Increase of

Stage Cross Current IPA Extracted
Experimental
Graphical

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Viva Questions
13. Express different notations and appropriate diagram of liquid-liquid equilibrium.
14. What is selectivity? Can you separate by liquid extraction if =1.
15. What are Tie lines & Plait points? Locate them in different diagrams.
16. The nature of the ternary diagram for completely miscible mixtures and partially
miscible mixtures will be same. True or false. If false sketch the nature of the diagram
for both the types.
17. Tie lines can be determined by (a) calculation (b) experimentally.
18. What is cross-current, co-current and counter-current operation in leaching, extraction
and adsorption operation.
19. What is the equilibrium line for leaching operations.
20. What is solute, solvent and diluents in an Liquid-Liquid Extraction

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Experiment No: 11 Date:

Hold up studies in the packed column

Aim: To determine the total hold up in the packed column

Apparatus: Packed column set up

Theory: Holdup refers to the liquid retained in the packed column. It may be due to wetting
the packing with liquid and pools caught in the crevices between packing materials. The
liquid holdup in packed columns is one of the significant parameters for the efficiency of unit
operations and processes. The column internals play a major role in the performance of a
packed bed reactor. Structured packings possess a high surface area. Packed columns are
widely used for solid catalyzed heterogeneous reactions and mass transfer operations.
Different packings are being tried for the efficiency of the operations. There are three
different types of liquid holdup namely Total holdup (ht), Static holdup (hs) ,and Operating
holdup (ho). The total holdup ht,is defined as the total liquid in the packing under operating
conditions. The static holdup is defined as the liquid in the packing which does not drain
from the packing when the liquid supply to the column is discontinued. The operating holdup
is defined as the liquid which continuously moves through the packing and replaced regularly
and rapidly by new liquid, represents the liquid which will drain from the packing when the
water flow is stopped.
The relation between the three holdups is given by:
ht = hs +ho

Procedure:
1) The equipment is made ready for operation.
2) The dry packing was thoroughly wetted by setting the water rate for around ten
minutes. Then the water rate was set to the desired value and the air rate was also set.
3) The water and air flow rates were kept constant for ten minutes before the operating
holdup was measured. This ensured a steady flow rate.
4) The time for collecting hold up was fixed at five minutes as it ensured complete
drainage. Simultaneously the manometer readings were recorded, and the water rate
was increased to the next higher value.
5) The different sets of packings of series of runs were made in the similar fashion with
and without air flows with increasing water rates.

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Observation & Calculation Steps:
AIR WATER SYSTEM
Berl Saddle –
Density of water at 28˚C = ρw
Volumetric flow rate of water ( R) = Mass flow rate of water (L0)
Area of packed column =

Operating Hold up

Volume of water held up

ho = -----------------------------------
Volume of packed column

Result:
Total holdup (ht) = ho + hg + hs + hst
Static holdup (hst), Solid holdp (hs) are assumed to be constant for a particular packing
hs = 0.390 m3 / m3
hst = 0.239 m3 / m3

Viva Questions
1. Why lower liquid hold up is preferred in packed bed distillation column?

2. Which are the different packing materials available commercially?

3. How the total liquid holdup varies with the liquid flow rate?

4. What is the importance of holdup studies?

5. What is the difference between packed column and tray column?

6. How do you calculate the packed column diameter?

7. What is the requirement of a good column packing?

8. how do you calculate the volume of packed bed?

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Experiment No: 12 Date:

Study the drying characteristics in the vacuum dryer

Aim: To study the drying characteristics by drying the given sample in a vacuum dryer.

Apparatus: Vacuum Dryer set up, stopwatch/clock

Theory: Drying is a simultaneous heat & mass transfer operation involving removal of moisture
from Wet solid by contacting with hot air. The air in turn gets humidified. If the solid is kept in a
chamber over a tray and air is passed over the plate/tray the dryer Is generally known as
Atmospheric Tray dryer. However more common type is Rotary dryer where wet solid and hot
air move through the inclined rotary dryer counter-currently, moisture from wet solid lost to hot
air. During drying, there are, generally, two stages of drying, constant rate and falling rate. In
the constant rate period, drying proceeds by diffusion of vapour from the saturated surface of the
solid across the air film. Moisture movement within the solid is rapid enough to maintain a
saturated condition at the surface and the rate of drying is controlled by the rate of heat transfer
rate to the evaporating surface. The mass transfer rate balances the heat transfer rate temp.
Humidity, velocity and direction of flow all remain constant and hence the name ‘constant rate
period. Once sufficient moisture is removed, rate continuously falls and this stage is called as
falling rate period. In some types of solids there are two falling rate period, first a linear rate
followed by a nonlinear period.

Procedure:
1) Take the sample (sand of dry solid) in the tray and note the weight.
2) Add known volume of water. Close the drying chamber’s door tightly.
3) Apply vacuum to the chamber and note the volume collected in the burette (= moisture
removed and condensed) and the time of collection.
4) Keep ice around the condenser tube to enable moisture to condense.
5) Observe volume and time till the volume is constant with time.
6) Repeat with different types of solid say, calcium carbonate.

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Observation & Data

Sl.No 1 2 3 4 5 6 7 8 9 10
Vol . (ml)
Time, sec

Diameter of tray , D = cm
Drying Area , A =  D 2/4 = [ m2 ]
Drying rate, N = dw/ (A)(dt) where dw = change in weight, = 2 gm or 2x 10-3 kg
Weight of dry solid w1= gm or w1x 10-3 kg.
Weight of moisture removed = volume of water collected.

Sl.No 1 2 3 4 5 6 7 8 9 10
-3
dw /dt x 10
kg /sec
N
[kg/( m2)sec)]
1/N 10-3

Specimen Calculation reading No. ----- -- .

Theoretical time of drying for removal of moisture from X1 to X2

ttotal = tc + tf where tc is time of constant rate period and tf is time of falling rate period

Ss (X1-Xc)
Time of constant rate period, tc = -----------
ANc

Ss
Time of falling rate period, tf = -* area under the
A curve of Fig. 3

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Result: Critical moisture content (from Fig.2) =

Equilibrium moisture content (from Fig.2) =
Theoretical time for drying =

Viva Questions
1) What are drying characteristics?
2) What are bound and unbound moisture, critical and equilibrium moisture content?
3) Saturated air will be used for drying wet material. True or false.
4) The maximum temperature attained by air during drying will be (a) equal to dry bulb
temperature (b) greater than dry bulb temperature (c) equal to wet bulb temperature (d)
greater than wet bulb temperature.
5) Explain the drying mechanism for different rate periods.
6) For identical condition of (inlet air, initial moisture content, Weight of dry solid, Surface
area). In which of the two i.e., atmospheric tray dryer and vacuum dryer you expect faster
rate of drying. Justify.
7) The moisture content of the dried material is (a) less than the critical moisture content (b)
equal to the critical moisture content (c) greater than the critical moisture content.

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Experiment No: 13 Date:

Determination of mass transfer coefficient by conducting wetted wall column experiment

Aim: To determine the mass transfer coefficient in a wetted wall column.

Introduction
A thin film of liquid falling down inside of a vertical pipe up through which the gas flows
constitutes a wetted column. Wetted wall columns have been used successfully as absorbers for
hydrochloric acid, ammonia, acetone, benzene and other volatile liquids. They have also been
used for theoretical studies for mass transfer, because the interfacial area between the phases is
kept under control and is measurable
Equipment
The all glass wetted wall column is used with the system air water to determine the gas film mass
transfer coefficient Kg. in determining the Kg the following auxiliary equipment is used.
Air blower
Rotameter for measuring water flow rate.
Two sets of wet and dry bulb thermometers.
Graduated cylinders and stop clock.
Inlet and outlet water temperature thermometers

Description
The figure enclosed shows the schematic of the wetted wall column experimental setup. The
inner diameter of the column is 25.4 mm and length of the column is 98 cm. Air is supplied to
the column at the bottom by means of blower. Bypass valve V1 and control valve V2 are used
for varying the air flow rate. Air flow rate is calculated by measuring the pressure drop across an
orifice meter fitted in the inlet air line. The orifice diameter is 5mm. The condition of air at inlet
and outlet of the column are measured by the wet and dry bulb thermometers WDB1 and WDB2
respectively. Water flow rate is measured by rotameter R1. The thermometers T1 and T2
measure inlet and outlet temperatures of water. A wire mesh screen is placed on top of the
column to distribute water uniformly over the surface of the tube. A water manometer M1
measures the pressure drop across column. A mercury manometer M2 measures pressure drop
across the orifice. Also a heating element is provided in the air inlet line so that air inlet
temperature can be varied if desired.
Theory
The measured flow 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 in the air from the water film and

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the resultant humidity of the exit air and the temperature and vapor pressure of the entry water is
measured. The rate of diffusion through the gas film NA is given by
NA Kg.mol/sec = Kg A(p)m
Kg = Gas film coefficient, Kg.mol.water transferred/m2.sec. partial pressure difference in N/m2.
A = wetted surface of column = dlm2
(p)m = log mean partial pressure driving force across the ends of the column.
This value of Kg obtained experimentally can then be compared with that predicterd from the
Sherwood Gilliland correlation.
Kg = (Dgd/RT).(dv/)0.8 (/Dg)0.44
Where d is column diameter.

Procedure
1) Water is fed at a rate at which complete wetting of the surface occurs and minimum
ripple formation is visible.
2) The blower is started, and a minimum flow of air is maintained.
3) After about ten minutes when steady conditions prevail, the humidity of air at inlet and
outlet are determined by the readings of the wet and dry bulb thermometers, using
Psychrometric chart. Water flow rate and inlet and outlet temperatures are recorded.
4) Use steam tables and find the vapor pressure of water at temperatures noted.
5) Calculations are made at different flow rates and values of Kg are plotted against
respective Reynold numbers (Re) on a log-log graph sheet.

Observations
INLET WATER CONDITIONS
Water flow rate is fixed such that complete wetting of column with a minimum of ripple
formation takes place.
Water flow rate as noted from rotameter = lpm.
Inlet water temperature is noted
This flow rate is maintained constant throughout and observations are noted for different air flow
rates.

AMBIENT AIR CONDITIONS

Ambient air dry bulb temperatures (DBT) = 0C

Ambient air wet bulb temperatures (WBT) = 0C
The above temperatures are noted using a dry bulb and wet bulb thermometer.

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Ambient air humidity is found from a humidity chart using the above temperatures. Apply
barometric correction to the humidity noted from the chart if the atmospheric pressure at the site
is not 760 mm Hg. For humidity correction factor please refer to perrys Chemical Engineers
Hand book VI edition, page no 20-7.

Observation table

S No Manometric Inlet Inlet Outlet Outlet Inlet Outlet

M2 reading Air Air Air Air Water Water
for air flow DBT WBT DBT DBT Temperature Temperature
rate Rm cm
1
2
3
4
5
6

CALCULATION:

Calculation of air flow rate

Orifice meter manometer reading, Rm=… ............. m.
Pressure drop, p= Rmg(m -a) N/m2.
Where
m is the density of the Manometric fluid(Hg).
a is the density of the process fluid (ambient air).

Calculation of a
Find density of ambient air is using ideal gas equation.

Calculation of velocity of air at orifice.

Vo=[0.61/(1-4)][{(2p)/a}]
Where  =do/dp(orifice diameter/pipe diameter).

Calculation of air mass flow rate

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ma =aVoAo Kg/sec
where
ma is mass flow rate of wet air in Kg/sec
Ao is crossectional area of orifice m2

Calculation of Ao
Ao=  do2/4.
Where
do is diameter of orifice m
Calculation of inlet air humidity
Get the humidity from the humidity chart using the dry bulb and wet bulb temperature of
ambient air.apply the humidity correction factor as mentioned before and get the actual humidity
at site .
Humidity of inlet air ,
Ha=…..Kg of water vapour/Kg of dry air(dry basis)
Humidity of inlet air ,
Ha=…..Kg of water vapour/Kg of wet air(wet basis)
Express ma as dry gas rate using the absolute humidity calculated above.

Ma=…..Kg of dry air /sec

Where Ma is the inlet dry air rate. That is Kg of bone dry air/sec
Calculation of exit air humidity
Get the humidity from the humidity chart using the dry and wet bulb temperature of exit air.
Apply the humidity correction factor as mentioned before and get the actual humidity of a exit
air at site condition .
Humidity of exit air,
He=……Kg of water vapour /Kg of dry air(dry basis)

Calculation of evaporation rate

Evaporation rate, Na=Ma(He-Ha)/18 Kg moles of water/sec.

Calculation of wetted surface of the column

Wetted surface of the column is given by A=dl. m2
Where d is the inner dia of column
l is the effective length of the column.

Calculation of (p)m

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Log mean partial pressure driving force across the ends of column is calculated as,
(p)m=(p1-p2)/ln(p1/p2).
p1=p*1-pw1
p*1=vapour pressure of water corresponding to outlet temperature of water N/m2
pw1=partial pressure of water vapour in inlet air in N/m2
Subscript 1 indicates the conditions at the bottom of the wetted column.
Where p2=p*2-pw2
P*2=vapour pressure of water corresponding to inlet temperature of water N/m2
Pw2=partial pressure of water vapour in exit air in N/m2
Subscript 2 indicates the condition at the top of the wetted column.
Vapour pressure data for water at different temperature is obtained from steam table. Calculation
of partial pressure of water vapour in air may be computed from the respective humidity values.

Calculation of mass transfer coefficient Kg

NA = KgA(p)m
Hence Kg = NA/[A((p)m] kgmoles water /sec.m2(N/M2)

Verification of application of sherwood Gilliland correlation.

Sherwood Gilliland correlation is,
Nsh = 0.023(Nre)0.8 (Nsc)0.44
Where Nsh is Sherwood number (Kg RTd)/Dg
Nre is Reynolds number (dG)/
Nsc is Schmidt number (/Dg)

G is mass velocity of air, G = v

V is velocity of air in the coumn
 is density of air at mean temperature
 is viscosity of air at mean temperature
R is univeral gas constant in appropriate units.

Dg is diffusivity of water vapor in air at experimental condition (at 273 K, 1 atm is 0.220 * 10-4
m2/s
Mean temperature is the arithmetic mean of inlet and outlet dry bulb temperatures of air.

Graphical representation of Gilliland Sherwood equation

(Nsh) = 0.023(Nre)0.8(Nsc)0.44

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(Nsh) (Nsc)-0.44=0.023(Nre)0.8
let Y be (Nsh)(Nsc)-0.44 and X is (Nre)
then equation 2 becomes
Y = Constant X0.8
When Y is plotted against X on log-log graph sheet it results a straight line making a slope of 0.8

Calculation of G
Mass velocity of air inside the column, G = (ma)/(d2/4) kgs.m2
Where ma is mass flow rate of wet air in kg/sec
D is the inner diameter of the column in m

Calculation of Dg at experimental condition

Use Dg1/Dg2 = [(T1/T2)3/2] [pt2/pt1]
Where Dg1 is diffusivity at temperature T1 and pressure pt1 (standard data from perry). Dg2 is
diffusivity at temperature T2 and pressure pt2 (experimental temperature and pressure)

Calculation table
Sl Rm ma G NA Kg Nsh Nsc Nre Y
no cm Kg/sec Kg/secm2 kgmoles/sec Kgmoles/sec
m2
1
2
3
4
5
6

Result: The mass transfer coefficient in a wetted wall column is found out.

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Viva Questions

1) What is wet and dry bulb Temperature?

2) How heat and mass transfer occur in wetted wall column.
3) What does Fick’s law state?
4) What are the different driving forces for diffusion?
5) What is the role of molecular diffusion in mass transfer?
6) What are different types of fluxes in mass transfer? Explain.
7) Explain Humidification and Dehumidification process with examples.
8) What is Mass Flux and explain its significance?

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Experiment No: 14 Date:

Measurement of cooling tower characteristic parameter

Aim: To determine the overall heat transfer coefficient in a forced draft counter current cooling
tower. To measure Tower Characteristic parameter KV/L for various liquid and airflow rates
(L/G) in a counter-current Forced draft Cooling Tower.
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 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 the cooling.
Theory:
Water may be cooled by the air if 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 heat 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. Assume that liquid is warmer than gas.
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.
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

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provided in airline 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 is
provided at both inlet and outlet of air stream. These sensors give Dry bulb & Wet bulb air
temperatures. The cooling tower is packed with Aluminum expanded wire mesh.

Experimental procedure:
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 & air flow rates within operational range.

CALCULATIONS:
Diameter of Orifice, mm (d1) =
Diameter of pipe, mm (d2) =
Coefficient of discharge Cd=

Density of manometer fluid w (kg/m3) =

Density of air, (kg/m3) =

g = 9.81 m/s2
Flow rate =
S. No. T1 T2 T3 T4 T5 T6 R1(cm) R2(cm) QW (LPH)
1
2
3

Calculations :

= m
a1 =Cross Section area of Orifice, m2= m
a2 = Cross Section area of pipe, m2 = m

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= m3/s

= kg/s

= kg/s

=
From Enthalpy table, the enthalpy of entering air at a wet bulb temp is h1= Btu/lb of air

= Btu/lb of air

T,0F hwi hai

T=T2 = hw = -------- ha = h1 = --------

T=T2 +0.1(T1-T2)= hw = ha = h1+0.1(L/G) (T5-T6) =
T=T2 +0.4(T1-T2)= hw = ha = h1+0.4(L/G)(T5-T6) =
T=T2 -0.4(T1-T2)= hw = ha = h2-0.4(L/G)(T5-T6)=
T=T2 -0.1(T1-T2)= hw = ha = h2-0.1(L/G)(T5-T6) =
T=T1 = hw = ha = h2 =

Cooling range = T5-T6 =

Temperature approach =T2-T6 =

=
Result:
The overall heat transfer coefficient in a forced draft counter current cooling tower is
determined.

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Viva Questions
1) Does the wet bulb temperature be greater than or lesser than dry bulb temperature?
2) What is adiabatic saturation temperature?
3) What is the role of molecular diffusion in mass transfer?
4) How heat and mass transfer operations are involved in cooling towers
5) What are the different type of cooling towers?
6) Mention the industries where cooling towers are used.

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Experiment No: 15 Date:

Solid Dissolution Studies

Aim: To determine (i) the specific rate of dissolution of Benzoic acid in sodium hydroxide
solution with instantaneous reaction and (ii) the dissolution transfer co- efficient for physical
dissolution of Benzoic acid in Deionzed water.

Apparatus: Moulds of different shapes, Dissolution set-up.

Chemicals: Benzoic Acid, Sodium Hydroxide, oxalic acid, phenolphthalein indicator,
distilled/deionised water.

Theory: Solid -liquid mass transfer plays an important role in many industrial operations. The
dissolution may be accompanied by a dissolved solid-liquid or dissolved solid-gas reaction. In
such cases, it is desirable to know the enhancement in the mass transfer due to instantaneous
reaction
→ A+2B Products. This reaction is considered as instantaneous
So that A and B cannot coexist. Species A dissolves in to the liquid phase and reacts with species
B diffusing from the bulk of the liquid at the reaction plane.
C6 H5COOH + NaOH C6 H5COONa + HOH
Thus for each mole of Benzoic acid dissolved and reacted one mole of sodium hydroxide is
consumed. The dissolution rate can, therefore, be followed by determining the fall of NaOH
concentration. The rate of dissolution of Benzoic acid is given by

[NaOH]i – [NaOH] f
R= x Volume of NaOH
Time

Where R is the rate of dissolution, [NaOH] i & [NaOH] f are initial and final sodium hydroxide
concentrations respectively. The specific rate of dissolution is then obtained by R’= R/Aav where
Aav is the average surface which is given by
Aav =  DavLav + 2 {/4(Dav2 - Dr2)}
KSL for physical dissolution is obtained from the integrated material balance for species A
KSL (ap/v )t = ln [1- (co/cw)]
Where ap = the cylinder surface area, m2 ; v = volume of solution, m3; t = time in sec;
co = bulk liquid concentration of Benzoic acid at time t sec. ; cw = solubility of Benzoic acid in
water = 0.0276 kmol/ m3

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Procedure:
1) Prepare the solid Benzoic acid by melting the acid and pouring in the cylindrical mold
with glass rod in the center.
2) Measure the dimensions of the cylinder.
3) Prepare 500 ml of 0.2N sodium hydroxide and 1 lit of 0.2 N oxalic acid.
4) Accurately standardize sodium hydroxide by titrating against standard oxalic acid using
phenolphthalein as indicator.
5) Take 250 ml of sodium hydroxide solution.
6) Fix the cylinder in the set up and start the motor and allow the dissolution to proceed for
20 minutes.
7) Stop the operation, mix the contents of the beaker and titrate samples against oxalic acid.
Measure the final dimensions of the cylinder.
8) Take an identical cylinder and immerse in distilled/deionized water and carry out
physical dissolution operation for time intervals of 20 min, 30 min, 40 min , 50 min.
9) Titrate samples of 10 ml at the end of each time intervals against standard sodium
hydroxide solution.
10) Repeat for different shapes of solid Benzoic acid.
Observations & Calculation Steps:
Dissolution with reaction
Weight of Oxalic acid required for 0.05N
Normality of NaOH [NaOH]i = gm mole/lit = kmol/m3
Dimensions of solid (cylinder)
Initial Dia Di = m
Initial length L i = m
Dia of glass rod, Dr = m
Final Dia, Df = m
Final length, Lf = m
Average Dia , Dav = (Di+ = Df )/2 = m
Average length, L av = (Li+ = Lf )/2 = m
Aav =  DavLav + 2 {/4(Dav2 - Dr2)} = m2
Volume of NaOH = 250 ml= 250*10-6 m3
Titre value (final) = ml
Final concentration [NaOH]f = 0.2*titre value(final)/(10)N
[NaOH]i – [NaOH] f
R = ------------------------------ x Volume of NaOH kmol/sec
Time (sec)
R’ = R/ Aav = = kmol/(m2)(sec)

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Physical Dissolution
Solubility of Benzoic acid, C w = 0.0276 kmol/m3

Time Volume of Co
Co/ Cw ln[(1- C o / C w)
(min) NaOH , (ml) ( Kmol/ m3 )
10
20
30
40
50
Volume, V = 250ml=250*10-6 m3
Ap =  DiLi + 2{/4(Di2- Dr 2)} = m2
C o=> (N*V)mix =(N*V)NaOH
C o=>Nmix =
Slope from a plot of Ln[(1- C o / C w) vs t = KSL (Ap/V ) and from slope
KSL = m/s

Result: Specific Dissolution rate, R’ = kmol/(m2)(sec)

Physical Dissolution Co-efficient , KSL = m/s

Viva Questions

13. Give different types of chemical reactions in mass transfer with chemical reactions.
14. What is solid dissolution?
15. Under what type of reaction your experiment in solid dissolution is based. What is the rate
determining step in such case?
16. Give practical examples of mass transfer with chemical reaction similar to your experiment
ie., solid dissolution.
17. What is deactivation of adsorbent?
18. What is regeneration of adsorbents?
19. What type of diffusion occurs in adsorption?
20. What is signification Specific Dissolution rate and Physical Dissolution Co-efficient?

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Experiment No: 16 Date:

Separation of DNA using Gel-Electrophoresis experiment

Aim: To separate DNA samples using Gel Electrophoresis.

Apparatus: Gel Electrophoresis kit
Theory:
Agarose gel electrophoresis is a method used in biochemistry and molecular biology to separate
DNA or RNA molecules by size. This is achieved by moving negatively charged nucleic acid
molecules through an agarose matrix with an electric field. Shorter molecules move faster and
migrate further than longer ones. Gel electrophoresis is a special technique that molecular
geneticists have developed in order to further research in biotechnology. The purpose of this
technique is to separate pieces of the DNA molecule by molecular size and shape.
You may recall from other science classes that the paper chromatography was used to
separate different molecules within a mixture (black ink, leaf pigments). In that method,
differences in the molecular weight and solubility of the molecules caused the molecules to rise
up the paper at different rates eventually resulting in their separation. Separation by
electrophoresis differs from chromatography in that the DNA molecules are moved by an
attraction to an electric charge and that the DNA must diffuse through a porous agarose gel.
A good analogy of a gel is a sponge, if you can imagine how large and small particles
would pass through a sponge at different rates according to particle size/shape verses the size of
the holes in the sponge. The rate of molecular movement depends upon molecule size/shape and
the direction of movement depends on the electric charge (+ or -) of the molecules, and the
density of the gel through which the DNA moves. Today, however, you will be separating
different color dyes, some have a positive charge and others a negative charge.
Materials: Agarose 0.5 X TBE,Weighing paper, Bromophenol blue
Equipment: Balance, Erlenmeyer flask, Microwave, Gel box with comb,UV Lamp
TBE- TBE stands for Tris Borate EDTA
People also use TAE (Tris Acetate EDTA). Make up a 10x stock using cheap reagents.
Do not use expensive ‘analytic grade’ reagents. Cheap Tris base and boric acid can be bought in
bulk.
Composition (10x solution)
Tris base 107.81 g/l (0.89 M)
EDTA 5.84 g/l, disodium EDTA dehydrate 7.44 g/l (0.02 M)
Boric acid 55.0 g/l (0.89 M)

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Preparation of Gel
There are several methods for preparing gels. A common example is shown here. Other
methods differ in the buffering system used, the sample size to be loaded, the total volume of the
gel (typically thickness is kept to a constant amount while length and breadth are varied as
needed). Most agarose gels used in a modern biochemistry and molecular biology are prepared
and run horizontally.
Make a 1% agarose solution in 100 ml TBE, for typical DNA fragments. A solution of upto 2-
4% can be used if you analyse small DNA molecules and for large molecules a solution as low as
0.7 % can be used.
Carefully bring the solution just to the boil to dissolve the agarose, preferably in a microwave
oven,
Let the solution cool down to about 60oC at room temperature or water bath. Stir or swirl the
solution while cooling. Wear gloves from here on, Ethidium bromide is a mutagen.
Add 5µl ethidium bromide stock (10mg/ml) per 100 ml gel solution for a final concentration of
0.5µg/ml.
Stir the solution to disperse the ethidium bromide then pour it into the gel rack.
Insert the comb at one side of the gel, about 5-10 mm from the end of the gel.
When the gel has cooled down and become solid, carefully remove the comb. The holes that
remain in the gel are the wells or slots.
Put the gel, together with the rack, into the tank with TBE. Ethidium bromide at the same
concentration can be added to the buffer. The gel must be completely covered with TBE, the
slots at the end electrode that will have the negative current.
Tips to improve the gels
Do not shake the gel chamber while loading as this will facilitate diffusion of samples out of the
wells.
Insert pipette tips at an angel to avoid puncturing the well which will result in loose of sample.
Always make sure that gel is running before leaving.
The longer the samples sit in the buffer, the more diffusion of bands can be visible. Always load
one row of sample at a time and run the gel for 5mins, then load the next row of samples. This
will minimize sample diffusion.

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Procedure
After the gel has been prepared, use a micropipette to inject about 2.5 µl of stained DNA
(a DNA ladder is also highly recommended). Close the lid of the electrophoresis chamber and
apply current (typically 100V for 30 minutes with 15 ml of gel). The colored dye in the DNA
ladder and DNA samples acts as a “front wave” that runs faster than the DNA itself. When the
“front Wave” approaches the end of the gel, the current is stopped. The DNA is stained with
ethidium bromide and is then visble under ultraviolet light.
The agarose gel with three slots/wells (S).
Injection of DNA ladder (molecular weight markers) into the first slot.
DNA ladder injected. Injection of samples into the second and third slot.
A current is applied. The DNA moves toward the positive anode due to the negative charges on
its phosphate backbone.
Small DNA strands move fast, large DNA strands move slowly through the gel. The DNA is not
normally visible during this process, so the marker dye is added to the DNA to avoid the DNA
being run entirely off the gel. The marker dye has a low molecular weight, and migrates faster
than the DNA, so as long as the marker has not run past the end of the gel, the DNA will still be
in the gel.
Add the color marker dye to the DNA ladder.
Result:
After electrophoresis the gel is illuminated with an ultraviolet lamp (usually by placing it
on a light box, while using protective gear to limit exposure to ultraviolet radiation) to view the
DNA bands. The ethidium bromide fluoresces reddish-orange in the presence of the purified
DNA. The gel can then be photographed usually with a digital or Polaroid camera. Although the
stained nucleic acid fluoresces reddish-orange, images are usually shown in black and white.

Viva Questions

5. What is gel electrophoresis?

6. What is the role of molecular diffusion in mass transfer?
7. What are steady state & unsteady state diffusion?
8. Name the applications of gel electrophoresis.
9. What is downstream processing?
10. What is the unit of diffusion Co-efficient and what are the analog terms in heat and
momentum transfer operations?
11. What are the different conditions under which diffusivity is determined? Give mass
transfer operation for each.
12. Under what condition you are conducting diffusivity experiment?

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Experiment No: 17 Date:

Casting of membrane
Aim:

To form a polyethersulfone (PES) membrane by unsteady state phase separation from a solution
of PES in N-methyl pyrrolidone (NMP) and to estimate the percent porosity of the membrane.
Apparatus:

16% Polyethersulfone (PES) dissolved in N-methyl pyrrolidone (NMP), Isotonic solution with
0.02 % sodium azide, Vitamin B12 1% in isotonic saline (B), hemoglobin 2% in isotonic saline
(C), Membrane Casting Apparatus, flat glass plate (one side rough), beakers , Mallet and die,
Torque wrench (variable moment) , conical flask (200 ml) , Graduated cylinder (50 ml)--2 ,
clamps , "doctor bar" , glass photograph developing dish.

Theory: Membrane are used in biotechnology, dairy, water treatment, nanomaterial industry for
processing of fine particles, colloids and biological materials such as protein precipitates and
microorganisms and separation of many other products. Transport through membranes depends
on its properties as well as those of fluid mixture and hydrodynamics. The separation may be
governed by size-exclusion or other interactions between the various components of the phases
and the membrane materials. The physical method measures the morphology related parameters
like pore shape, size, its distribution, membrane thickness and porosity.

Procedure:
1. The following procedure is to be repeated a few times to obtain at least two good films from
the 16 % PES solution.
2. Set the doctor bar on the glass plate's rough side with 0.007 inch clearance down, so gap is
0.007 inch. Snap in the aluminum guards so that a rectangular reservoir is defined between it, the
glass plate, and the doctor bar. Attach the end guide with a 1/4-20 machine screw so that as the
end guide slides along the 10-inch side of the 8 X 10 glass plate, the doctor bar moves at 90
degrees to the 10-inch side. Start with the doctor bar close to an 8-inch side of the glass plate.
3. Dispense about 20 ml of the PES-NMP solution into a beaker. Then from the beaker pour the
solution slowly and uniformly into the rectangular reservoir. Avoid entraining air.

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4. Place paper towels under the far end (8 inch wide end) to catch excess solution. Move the
doctor bar with a uniform motion about 1 inch per second, so that it spreads the solution over the
glass plate as a uniform layer. Keep moving until the doctor bar, guard, and end guide go off the
glass plate and onto the paper towels.
5. The PES-NMP liquid film on the glass plate is now ready for conversion to membrane by
immersion in a tray of water.
6. The doctor bar and its attachments are cleaned up under running water which precipitates the
PES. The NMP is safely discharged in the waste water. When the glass plate is retrieved from
the tray of water, the membrane will have floated cleanly off.
7. The membrane porosity is the total void volume present within the membrane and is
commonly defined as the pore volume divided by the total volume of the membrane:
8. The porosity of the membrane was calculated using the average mass of the polymer material
and the mass of liquid in the membrane. The volume of the membrane was determined
gravimetrically by weighing a sample of known area and thickness. The density of the membrane
polymer material was noted from literature. The membrane thickness was determined by a digital
micrometer.
9. The porosity of the membranes was calculated using the equation:

Result: Porosity of the membrane

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Viva Questions
1. What is the role of temperature in membrane structure and formation?
2. What are the different types of membrane separations?
3. What is the difference between the filtration and membrane separation?
4. what is solution casting method?

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