National Institute of Technology

Tiruchirappalli-620 015

Department of Chemical Engineering

Mass Transfer
Laboratory Manual

Chemical Engineering Department, NIT Trichy

Page 1

List of Experiments
1) Determination of diffusion coefficient. Studies on
determination of Diffusion coefficient for Acetone in air and
Mass transfer coefficient for Naphthalene in Air
2) Verification of Rayleighs equation
3) Determination of optimum number of stages for Leaching
4) Determination of thermal and vaporization efficiency in
steam distillation
5) Verification of Freudlich Adsorption Isotherm
6) Studies on Air Drying and determination of drying
characteristics
7) Studies on Vacuum Drying and determination of
drying characteristics
8) Determination of Mass transfer coefficient using Wetted Wall
column
9) Determination of mass transfer coefficient in Surface

Evaporation

Chemical Engineering Department, NIT Trichy

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1. Studies on determination of Diffusion coefficient for Acetone in air and Mass

transfer coefficient for Naphthalene in Air
Aim: To determine the diffusion coefficient of acetone in air and Naphthalene in air
Theory:
Diffusion is the net movement of molecules or atoms from the region of high
concentration (high chemical potential) to a region of low concentration (low
chemical potential). This is also referred to as the movement of a substance down a
concentration gradient.
Ficks Law of Diffusion:
The diffusivity or diffusion coefficient DAB of a constituent A in solution B,
which is measure of its diffusive mobility, is then defined as ratio of its flux to its
concentration gradient.

There are two types of diffusion:

1. Molecular Diffusion
2. Eddy Diffusion/ Turbulent Diffusion
1. Molecular Diffusion:
Molecular diffusion is concerned with the moment of individual molecules
through a substance by virtue of its thermal energy. The driving force for this
diffusion is concentration gradient.
2. Eddy Diffusion/ Turbulent Diffusion:
Eddy diffusion is a process where substances present in the fluid system are
mixed by a simple agitator to achieve a complete uniformity, this mechanical agitation
produces rapid movement of relatively large chunks or eddies of fluid characteristic
turbulent motion.

Chemical Engineering Department, NIT Trichy

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Procedure:
Liquid in Air Diffusion:
Acetone is taken in a long column and air is passed over the liquid. The
change in the liquid level with respect to time is noted. From this, diffusion rate is
estimated and the diffusivity is determined.
Formulae:
Winkle Manns Method:

From the plot of

vs

, slope can be formed out and the diffusivity

can be calculated.
Solid in Air Diffusion:
In this method naphthalene is taken in a long cylinder and air is passed through
the cylinder. The change in weight with respect to time is noted. From this diffusion
rate is estimated, and diffusivity is determined.

Chemical Engineering Department, NIT Trichy

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Formulae:

Where,

From the plot of

vs

, we get a relation between

From plot,

Where

Chemical Engineering Department, NIT Trichy

Page 5

2. Verification of Rayleighs equation

Aim:
To verify Rayleigh equation and to determine the relative volatility.
Theory:
Simple distillation is a mass transfer operation for the separation of a
component from a mixture, wherein a new phase is created by supplying heat to the
liquid phase. The new phase is created by continuous heat supply. The more volatile
component is predominantly present in the vapour phase. Its usually applied in
removing gum from agents from oil extracts.
F
xf dx

y x
ln W
xw

Procedure:
150 ml of 50 mol% isopropanol and water solution is taken in a round
bottomed flask. The flask is progressively heated and the vapours formed are
collected and condensed in a conical flask. About 70 ml of distillate is collected. The
composition of residue is determined by measuring its density and using a calibration
chart drawn density vs mol. fraction of more volatile component.

y
x
1
yx
Feed:
Specific gravity of isopropanol

Weight of feed + bottle

Weight of feed

Weight of bottle

Volume% of isopropanol in feed

Weight of water

Chemical Engineering Department, NIT Trichy

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Moles of isopropanol

Moles of water

Residue and distillate:

Specific gravity of residue

Specific gravity of distillate

Weight of residue + bottle

Weight of residue

Weight of distillate + bottle

Weight of distillate

Moles of isopropanol in distillate

Moles of water in residue

Area under the curve: (1/y-x) vs x

xf

dx

y x = ln F/W

Theoretically determined =

xw

FxF

ln

Obtain

WxW

F1 x

ln

W1

xW

Experimental Value of ln F can be determined

W
Compare the experimental and theoretical values.

Chemical Engineering Department, NIT Trichy

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3. Determination of optimum number of stages for Leaching

Aim:
To separate a solute constituent from a solid mixture by single stage and
multistage extraction with a solvent and to find out the percentage performance of
extraction.
Theory:
Leaching is preferential separation of one or more constituents of a solid
mixture by contact with a liquid solvent. Leaching differs slightly from the washing of
filtered solids and leaching equipment strongly resembles the washing section of
various filters. In leaching, the amount of soluble material removed, is often greater
than in ordinary filtration, washing and the properties of the solids may change
considerably during leaching operation.
Procedure:
The experiment is, leaching of NaOH from NaOH+Sand mixture, using water
as solvent, which is kept constant at 100ml. The experiment is carried out in different
stages.
10 g of sand and 2 grams of NaOH is taken in 5 beakers. Water (100ml) is
added to each of the beakers in different sages such as one, two, three four and five
stages. The total stirring time is constant. The composited extract from each stage is
titrated against Oxalic acid, to determine the percentage extraction of NaOH.

Tabulation:
S.No.

No. of stages

Volume of Volume of NaOH

extract
consumed

Normality
of NaOH

Extraction
efficiency

Formula:
% Extraction =

Volume of NaOH consumed at any stage 100

Volume of NaOH consumed at infinite stage

Chemical Engineering Department, NIT Trichy

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4. DETERMINATION OF THERMAL AND VAPORISATION

EFFICIENCY IN STEAM DISTILLATION
Aim: To conduct an experiment on steam distillation and to determine the
thermal efficiency and vapourization efficiency.
Theory:
Insoluble liquids distilled with steam can be made to boil at a
temperature much lower than the boiling point of water. This method is
adopted when the substance decomposes at higher temperature. In steam
distillation, the sum of vapor pressures of components equal to total pressure,
then the mixture starts to boil at constant temperature till one of the
components completely get vaporized without decomposing the another high
boiling component.
Pt = P A + PB
Procedure:
150 ml of aniline is taken and steam is bubbled. About 100ml of
distillate is collected and allowed to cool. Aniline and water are separated
using a separating funnel. The residue and distillate are obtained and the
volume is determined.
Tabulation:
Aniline
Vapour Pressure
mmHg

Water
Temperature
C

Vapour Pressure
mmHg

Temperature
C

Calculation:
Initial volume of aniline

Volume of aniline in distillate

Volume of water in distillate

Volume of aniline in residue

Volume of water in residue

Formula:

Chemical Engineering Department, NIT Trichy

Page 9

Reduced temperature TR1 actual temperature of aniline

critical temperature of aniline
Heat input mss msCPs(TP TR)
Heat output mss msCPs(TP TR)
Thermal efficiency Output 100
input
MA, D
Vaporisation Efficiency

MW, D

MW of Aniline Vapour pressure of aniline

Vapour pressure of Water

100

MW of Water

Chemical Engineering Department, NIT Trichy

Page 10

5.Verification of Freudlich Adsorption Isotherm

Aim:
To study the adsorption of oxalic acid on charcoal and to verify the
Freundlich adsorption isotherm.
Theory:
The adsorption operation explains the ability of certain solids to
preferentially concentrate specific substances from solution. In these operations,
there is an equal distribution of the original constituent between adsorption phase
at the surface and the bulk of the liquid, thus permitting separation to be made.
According to the Freundlich equation,
Y = m Xn
where,
Y = mass of solute / mass of
solvent X = mass of solute / mass
of adsorbent
Procedure :
Prepare 0.5 N Oxalic acid and 0.2 N NaOH. Take 2g of charcoal in 5
different reagent bottles. Add 20, 30, 40, 50 and 60 ml of oxalic acid and make it
to 100 ml using water. Shake it well for 30 min and then filter it. Filtrate is
titrated against NaOH to get the amount of oxalic acid remaining in the flask.
Tabulation:
S.No. Volume of Titre value
(COOH)2 ml
ml

Y
Kg solute
Kg solvent

- lnX

- lnY

Kg solute
Kg adsorbent

Formula:
Initial Normality of oxalic acid, N(COOH) = 0.5 and NNaOH = 0.2
N(COOH)final

(V N)NaOH

V(COOH)
Initial amount of oxalic acid present (20 ml) = (0.5 63.5 20)/
1000 gms Amount of oxalic acid present in the filtrate (100 ml)
= {N(COOH)
63.5100}/1000 gms Amount adsorbed
= Initial Final
X = Amount adsorbed /2
2

Chemical Engineering Department, NIT Trichy

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Y = Amount adsorbed / 100

From graph (lnY vs ln X), Slope m and intercept n can be determined.
Then establish a relation,
Y = m Xn

Chemical Engineering Department, NIT Trichy

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6. Studies on Air Drying and determination of drying

characteristics

Aim:
To estimate the drying characteristics of a given specimen and to
determine the mass transfer coefficient.
Theory:
Air is used as a drying medium in this experiment. Air is allowed to pass
over the wetted specimen. As a result, air gets humidified and the wet substance
gets dried. The drying rate characteristics are estimated during the constant rate
period. The rate of drying during the period is given by,
NC = Ky
(ys y)
Where,
y, ys are saturated humidity at the surface and
surrounding air Ky is the mass transfer coefficient
Procedure:
The specimen is wetted by soaking in water. It is weighed and kept in an
air chamber. Air is passed over it at an interval of 10 minutes. The weight of the
substance is measured periodically till the weight remains constant.
Tabulation:
S.No

T Temperature Weight of Time

(sand
+ (min.)
H2O + pan)

X W W0
W0

dX
dt

SS dX
.

A dt

Formula:
Nc Ss dx
A dt
H

ps MA
pt ps M B

y'

pi s MH20
760 - pi s Mair

X W W0
W0

Chemical Engineering Department, NIT Trichy

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NC

1 dW

, A-Area of transfer

A dt
NC
Ky PS Pi S
From plot, W vs t, dw/dt determined. Then drying rate vs moisture content is drawn to
determine the critical moisture content, Nc and Ky

Chemical Engineering Department, NIT Trichy

Page 14

7. Studies on Vacuum Drying and determination of drying characteristics

Aim:
To study the drying characteristics of a material under vacuum and to
determine the overall mass transfer coefficient using constant rate period.
Theory:
When the solid material dries, two fundamental processes occur.

Transfer of heat to evaporate liquids.

Transfer of mass as internal moisture.

Each process determines the rate of drying process. However, regarding the heat
transfer mechanism, The heat must flow first to the outer surface and then inside
surface and then inside .
Drying rate [Ss/A][dX/dt] where A is the area of drying surface.
Procedure:
A sample of given material, is prepared with a known moisture content.
The mixture is prepared uniformly and spread on a tray. The thermometer is
placed to measure the surface temperature. The vacuum is broken after 10
minutes and the shelf is opened and the tray is weighed quickly. This is repeated
for various intervals and the graph is plotted.
Tabulation:
S.No

T Temperature Weight of Time

(sand
+ (min.)
H2O + pan)

X W W0
W0

dX
dt

SS dX
.

A dt

Formula:
2
1) Area D
4

2) Pis TP Absolute Humidity

1 Absolute Humidity
NC
3) Ky PS Pi S
From plot, W vs t, dw/dt determined. Then drying rate Vs moisture content is drawn
to determine the critical moisture content, Nc and Ky
Chemical Engineering Department, NIT Trichy

Page 15

8. Determination of Mass transfer coefficient using Wetted Wall column

Aim:
To determine the mass transfer coefficient for air-water system in a wetted
wall column.
Theory:
A thin film of liquid running down the inside of a vertical tube with gas
flowing either cocurrently or counter currently, constitutes a wetted wall column.
Water tube devices have also been used for diffusion where the liquid film is
generated at the top by partial condensation so that interphase mass transfer occurs.
Procedure:
Water flow rate is fixed at a particular value. The air flow rate is varied and
(y)ln ln ln
S.No. Rotameter % Exit
Air
Flow NA
Absolute GS
NA (y) humidity
reading
Humidity flow
rate (Kg/hr)
of air
rate
(Kg/hr)
measured using a rotameter. For every flow rate, the exit humidity is measured and
tabulated.
Formula:
1) Dry air relative humidity = Inlet air humidity
2) Partial pressure = Relative humidity Vapour pressure at DBT
pp
MH2O
3) Absolute humidity =

TP pp Mair
4) Yin = (PPin/Pt PP) (18/28.84)
5) Yout = (PPexit/Pt PP) (18/28.84)
GWS
6) GS 1 Absolute Humidity
7) Area = DL
8) NA GS(yout yin)
DL
9) yln yi yin yi yout

ln

i
y

in
y

yi yout

Chemical Engineering Department, NIT Trichy

Page 16

From the plot lnNA vs ln(Y)ln , slope m and intercept n can be determined and
established a relation

NA = m (Y)lnn

Chemical Engineering Department, NIT Trichy

Page 17

9. Determination of mass transfer coefficient in Surface Evaporation

Aim:
To determine the mass transfer coefficient and to study the surface
evaporation phenomena.
Theory:
When vapour pressure of water at a particular temperature is higher than the
particular pressure of water vapour in the surrounding air, the evaporation takes
place. If the difference in them is made higher, then the rate of evaporation
increases.
Procedure:
A container with some water is suspended in a water bath maintained at a
particular temperature. The container is directly connected to a physical balance.
As soon as the temperature of the container reaches a particular temperature, the
stop clock is switched on and the time taken to evaporate 1g of water is noted. The
experiment is repeated. DBT and WBT of the surrounding is noted to estimate the
humidity of water vapour in air.
Tabulation:
S.No.

Bath
temperature
(C)

Timefor
Vapour
evaporation pressure
(sec.)
(mm Hg)

NA
g/cm2s 10-3

ln(PS P)

- ln NA

Formula:
1) Partial pressure = Vapour pressure humidity
2) Area

D 2
4

3) NA Rate of Evaporation Flux

A
Area Exposed
4) NA K(PS P)n
A
5) NA Rate
Area
6) Rate 1 gm of water
Time taken
From the plot (ln NA vs PS P), slope K and intercept n can be determined and
the relation can be established NA = Kp (PS P)n
Chemical Engineering Department, NIT Trichy

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