EXPT:

DATE:
DIFFUSIVITY OF VAPOUR IN GAS
AIM:
To determine the diffusion coefficient, or diffusivity, of the given vapor in gas.
THEORY:

The rates of mass transfer in operations such as humidification, desorption etc., are greatly
influenced by the diffusivity of vapor in a gas. Diffusivity measurement of vapour in gas is done
by Stefans experiment which is based on the pseudo-steady state diffusion in which one of the
boundaries (liquid-vapour interface) shifts with time and the other (vapour-gas interface) remains
constant. As a result, the length of the diffusion path changes with time. However, the change is
too slow to be considered as unsteady state. Hence it is pseudo-steady state diffusion of vapour in
gas and Stefans equation applies.
Stefans Experiment: The apparatus consists of a constant temperature bath in which a capillary
tube is
immersed. The open end of the tube is exposed to flow of a gas (B). The tube is filled with pure
liquid (A) to a certain level. Care is taken to see that the liquid column in the capillary is
completely immersed in the bath so that its temperature constant throughout the experiment. At the
start of the experiment the liquid level is observed by means of the spectrometer. The liquid being
a volatile one vapourizes and the vapour reaching the open end of the capillary tube diffuses
through the gas stream. As a result, the liquid level decreases with time and this is noted down.
AT STEADY STATE, IN GAS PHASE, FOR DIFFUSION OF A THROUGH NON-DIFFUSING B,

DIFFUSION COEFFICIENT FOR LIQUID-LIQUID SYSTEM

Expt:
Date:

AIM:
To determine the diffusion coefficient for NaOH in Water.

THEORY:
Diffusion - the process by which molecules spread from areas of high concentration, to areas of
low concentration. When the molecules are even throughout a space - it is called equilibrium.
Concentration gradient is defined as a difference between concentrations in a space.
Diffusion is the transport of a material or chemical by molecular motion. If molecules of a
chemical are present in an apparently motionless fluid, they will exhibit microscopic erratic
motions due to being randomly struck by other molecules in the fluid. Individual particles or
molecules will follow paths sometimes known as "random walks."
In such processes, a chemical initially concentrated in one area will disperse. That is, there will be
a net transport of that chemical from regions of high concentration to regions of low concentration.
An analogous form of diffusion is called conduction. In this case, heat is the "chemical" that is
transported by molecular motion. As in chemical diffusion, heat migrates from regions of high heat
to regions of low heat. The mathematics describing both conduction and diffusion are the same.
Most of the mass transfer operations used for separating the components of a solution achieves this
result by bringing the solution to be separated into contact with another insoluble phase. As will be
developed, the rate at which a component is then transferred from one phase to the other depends
upon a so called mass transfer or rate, coefficient and upon the degree of departure of the system
from equilibrium. The transfer stops when equilibrium is attained.
Although the liquid diffusion coefficient of a salt is known to vary with concentration, at relatively
low concentrations Ficks Law of diffusion can be said to apply in the form,
Dc / d = D / (d2c / dx2)
The integral form of this equation is normally expressed as,
N / (A) = (DL /) (C1 - C2)
N/

= Mass transferred per unit time

A
C1, C2
DL

= Area of transfer or contact

= Initial and Final concentration along transfer path
= Liquid Diffusion Coefficient
= Effective Film Thickness

In the cell the initial concentration = C1 and the initial concentration of the solute in solvent outside
the cell is 0. The final concentration in the cell is C2 and that in the solvent outside C3.
(C 0) (C2 C3 )
Then, C1 - C2 = (C)m = 1
C1
ln

C2 C 3
The diffusion can be considered as through an element dx of the strip of the cell.
X

Then

(N /)

dX = DL

(C)m

(N / ) X = DL (C)m
DL = N X / (C)m

PROCEDURE:
1. A small volume of concentrated solution (0.5 N NaOH) was placed on one side of the
honeycomb, whilst the other side initially consisted of a large volume of pure solvent (deionized water).
2. As the diffusion of the solute occurred, the concentration within the larger volume
increases.
3. The mixture was continually stirred to ensure uniform concentration within the bulk liquid.
4. The diffusion was allowed to take place for 30 minutes.
5. 20 ml of sample from the larger volume was pipetted out and titrated against standard HCl
using phenolphthalein as indicator.
6. 20 ml of sample from the smaller volume on the other side of the honeycomb was pipetted
out and titrated against standard HCl using phenolphthalein as indicator.
7. In both cases the end point was the disappearance of the pink colour.
8. From the Normalities of the two solutions the amount of solute that diffused is found out.
9. Consequently the diffusion coefficient of the solute in water was found out.

Observations:

Weight of NaOH pellets, w1

Volume of distilled water
Initial volume of cell solution

=
=
= Vin =

g
ml
ml

Normality of cell solution before diffusion NI in =

Final volume of cell solution

Time of operation

ml
s

= Vf =
=

Estimation of strength of NaOH solution:

NaOH vs HCl:
Indicator: Phenolphthalein
End point: Disappearance of pink color
A. Inner solution before diffusion:
NaOH vs 0.5 N HCl:
S.No

Volume of
NaOH solution
ml

Burette reading
Initial
Final

Volume of HCl
ml

Concordant value =
ml HCl
Normality of inner solution, NI in = VHCl NHCl / VNaOH =
=
B. Inner solution after diffusion:
NaOH vs 0.5 N HCl:
S.No

Volume of
NaOH solution
ml

Burette reading
Initial
Final

Volume of HCl
ml

Concordant value =
ml HCl
Normality of inner solution, NI f = VHCl NHCl / VNaOH =
=
C. Outer solution after diffusion:
NaOH vs 0.1 N HCl:
S.No

Volume of
NaOH solution
ml

Burette reading
Initial
Final

Volume of HCl
ml

Concordant value =
ml HCl
Normality of inner solution, NII f = VHCl NHCl / VNaOH =
=
Cin = NI in 0 =
Cf = NI f - NII f =
x = 0.001 m
Cin
------- =
x

NA

gmol / l
gmol / l

gmol/lm

Cin
= DAB ---------x

DAB = NA /

Cin
------x

moles transferred
m
NA = ---------------------- = -----at
Area x time
Initial moles = NI in x Vin =

gmoles

Final moles = NIf x Vf =

gmoles

M = Initial moles final moles =

gmoles

a = Area of contact = Do 2 / 4

m2 (Do = 1 cm)

Mass transferred = NA =
DAB =

RESULT:
An experiment was conducted on the liquid-liquid diffusion apparatus and the diffusion coefficient
for the NaOH-water system was found to be DAB

WETTED WALL COLUMN

Expt:
Date:
AIM:
To study the rates and phenomena of diffusion into gases flowing through the pipe and also
to verify the Sherwood & Gilliland correlations.
THEORY:

The chemical industry affords numerous examples of processes in which a gas is dissolved
by a liquid and then undergoes a chemical reaction in the liquid phase. For example, in the contact
process for the manufacture of sulfuric acid the sulfur trioxide formed by the catalytic oxidation of
sulfur dioxide is absorbed in a mixture of sulfuric acid and water with which it reacts chemically to
produce more sulfuric acid. Similarly the nitrogen oxides formed by the catalytic oxidation of
ammonia are absorbed in water and react to from nitric acid. In some cases an unwanted impurity
in a gas is removed by scrubbing with a liquid capable of reacting with it, as in the removal of
sulfur dioxide from flue gas by absorption in an alkaline solution or a suspension of slaked lime.
The separation and recovery of one constituent of a gas mixture may be effected by absorption in
liquor with which it undergoes a reversible chemical reaction. For example carbon dioxide is
removed from gases by absorption in mono-or diethanolamine, with which it reacts to form
carbonates, and subsequently recovered by heating the solution. The regenerated amine is then
returned to the absorption plant. In this case the advantage over a process involving physical
solution, e.g. in water, is the much higher solubility of carbon dioxide in the amine and the
consequent reduction in the rate of circulation of liquid through the absorber and regenerator.
The effect of a chemical reaction in the liquid phase is to increase the solubility of the
absorbed component and reduce its equilibrium partial pressure. If the chemical reaction is
irreversible, the equilibrium partial pressure is zero as long as any free reactant remains in the
liquid phase. Since the molecules of absorbed component must diffuse into the liquid phase until
they meet the reactant, and after the reaction, the product must diffuse into the bulk of the liquid,
the rate of absorption must depend on the concentration and diffusivities of the reactant and
products, on the rate of chemical reaction and on the depth of the liquid film in which the reaction
occurs.
PROCEDURE:
1. The water tank was filled with fresh tap water and the pump was switched ON by keeping
the bypass valve totally open.
2. The valve on the water rotameter was opened to adjust the flowrate of water through the
column and if no flow was obtained, the bypass valve was closed to get the desired flow of
water through rotameter. (Initially high flow rate of water was kept to obtain uniform

distribution of water throughout the perimeter of the column and then it was adjusted to the
desired level).
3. The Air compressor was switched ON and the rotameter valve was opened to set the flow
rate of the air at the desired value.
4. The Dry bulb and Wet bulb temperatures indicated by the thermometers located at the top
and bottom of the column were measured after 5 minutes.
5. The water flow rate and the air flow rate were changed to change the conditions of
humidity and /or turbulence. 4-5 readings of different nature were taken.

Observations & Calculations :

Flow rates:
Air flow rate
= QA =
Water flow rate = QW =

m3 /s
LPM

Temperatures:
Air temperatures
DBT, c
WBT, 0 c
TD1=
TW1=
TD2=
TW2=
0

Inlet
Outlet

Water temperature
0
c
T2 =
T1 =

Humidity Calculations:
At terminal 1:
W ( YW Y)
TD1 - TW1 = -------------------------hG / kY
W = latent heat of vaporization of water at TW1 in K
hG / kY = 0.95 KJ / Kg K
YW = YW at TW1
(TD1 - TW1) (0.95)
Humidity of air at inlet = Y1 = YW - ----------------------------W
=
=

Kg water vapor/ Kg dry air

10

At terminal 2:
TD2 - TW2 =

W ( YW Y)
-------------------------hG / kY

W = latent heat of vaporization of water at TW2 in K

hG / kY = 0.95 KJ / Kg K
YW = YW at TW2
(TD2 - TW2) (0.95)
Humidity of air at outlet = Y2 = YW - ----------------------------W
=

Y1 = YW1 -- Y1
=

Y2 = YW2 -- Y2
=

YAv =

Y1 + Y2
---------------2

Kg water vapor/ Kg dry air

Air flow rate in Kmol / s:

QA
273
Q = --------------- x ----------22.41
273 + TAv

TD1 + TD2
where TAv = --------------- =
2

Kmol / s

Humidity in Kmol water vapor / Kmol dry air:

Y2 = Y2 x 29 / 18 =
Y1 = Y1 x 29 / 18 =
Y1
y1 = ----------1 + Y1

11

Y2
y2 = ----------1 + Y2
y1 + y2
----------------2
Mass transfer rate NW= Q ( Y2 Y1 ) =
=
Kmol / s
NW
Mass transfer rate NW = ----- =
A
=
kmol/m2 s
ym =

NW
kY = ------------- =
ym
=
kY
kG = ------------ =
pt
=
RESULT:
An experiment was conducted on the wetted wall column apparatus and the rates and phenomena
of diffusion into gases flowing through the pipe were studied and also the Sherwood & Gilliland
correlations were verified.

12

SIMPLE DISTILLATION
Expt:
Date:

AIM:
To verify Rayleighs equation through simple distillation process..

THEORY:

The simplest form of a batch still consists of a vessel (pot or kettle) fitted with a heating
device, a condenser and a receiver. Feed is charged into the vessel, boiled slowly, and the vapours
are withdrawn as rapidly as they form to the condenser, where they are liquefied, and the
condensate (distillate) is collected in the receiver. The first portion of the distillate will be the
richest in the more volatile substance and as distillation proceeds, the vaporized product becomes
leaner. The distillate can therefore be collected in several separate batches, called cuts, to give a
series of distilled products of various purities. This process is often referred to as Rayleigh
distillation.
For a binary mixture, assuming that at any time during the course of distillation there are L
moles of liquid with x mole fraction of the more volatile component, and that V moles with y
mole fraction are vapourised, a material balance yields
-- y dV = d (Lx) .(1)
Assuming that the vapours issuing any time are in equilibrium with the liquid from which it
rises, equation (1) on rearranging and integration gives
F
dx
ln ----- =
----------------- ..(2)
W
y* -- x
where F represents the initial feed and W , the final residue left in the vessel, both in moles. The
RHS of the equation is evaluated by plotting 1/(y-x) vs x and measuring the area under the curve
between the limits xw and xF. If the mixture is a binary system for which relative volatility, is
constant or an average value be found for the range considered, then the LHS of equation (2)
can be calculated directly without the need for graphical integration.

y* / (1-y* )
= -------------------- (3)
x / (1-x)
F
ln ----W

1
xF (1 xW )
1 xW
---------- ln --------------- + ln ----------- ..(4)
-1
xW (1 xF )
1 xF

13

PROCEDURE:
1.150 ml of feed was prepared by mixing 100 ml of acetone and 50 ml of water.
2. The density of the feed solution was determined.
3. The distillation flask was charged with the feed and distillation started.
4. After collecting a considerable amount of distillate, the volumes of the distillate and the
residue were determined.
5. The densities of the distillate and the residue were determined.
6. The densities of at least 5 sets of A-B mixtures of varying compositions were determined
to obtain a density versus composition chart.
7. From the chart, the mole fraction of A in the residue (xW).and in the feed (xf) were
determined.
8. Rayleighs equation was verified.

Observation:
Compound A: Acetone
Compound B : Water
Density vs mole fraction, x data:
Density of A (acetone) = A
Density of B (water )
= B
Measurements are at room temperature.

Mixture Vol. of
acetone,
ml
I
II
III
IV
V
VI

10
8
6
4
2
0

Vol of
water
ml

Mole
Fraction
of A

Empty
sp.gr.
bottle

Mass,g
Vol. of
Sp. gr. Sample Sample,
ml
bottle+ taken
sample

Density,
g / cc

0
2
4
6
8
10

14

Feed
Volume of
methanol, ml
Volume of
Water, ml
Total volume,
ml
Density, g / cc
Mol.fraction of
A
No. of moles

Distillate

Residue

VF =

VD =

VW =

xF =

xD =

xW =

F=

D=

W=

Model Calculations:
Estimation of density & mole fraction, xA :
Density = Mass / volume
For mixture II:
8 ml
Volume of acetone, VA =
Volume of water,
VB =
2 ml
Mass of methanol, mA=
VA x A =
g
Mass of water,
mB =
VB x B =
g
Mol.wt of acetonel, MA=
Mol.wt of water,
MB=
18
No.of moles of methanol.=
mA / MA = nA
No.of moles of water
.=
mB / MB = nB
Mole fraction, xA
=
nA / (nA + nB )
Feed:
Volume of feed
= VF =
ml
Density of feed
= F =
g / cc
Average mol.wt. of feed = MF = MA xF + MB( 1- xF)
Mass of feed
= mF = VF x F =
g
Moles of feed
= F = mF / M F =
Residue:
Volume of residue
=
Density of residue
=
Average mol.wt. of residue =
Mass of residue
=
Moles of residue
=

VW =
ml
W =
g / cc
MW = MA xW + MB( 1- xW)
mW = VW x W =
g
F = mW / MW =

15

FORMULAE:
Rayleighs equation:
F
ln ----W

Relative volatility =

F
ln ----W

dx
----------------y* -- x
y* / (1-y* )
= --------------------
x / (1-x)

1
xF (1 xW )
1 xW
---------- ln --------------- + ln -----------1
xW (1 xF )
1 xF

Where F = moles of feed

W = moles of residue
xF = mole fraction of more volatile component in feed
xW = mole fraction of more volatile component in residue
F
ln ----W

Graph:
x versus

dx
--------y* -- x

1
xF (1 xW )
1 xW
---------- ln --------------- + ln -----------1
xW (1 xF )
1 xF
1
-----------y* - x

(from graph)

RESULT:
An experiment was conducted with simple distillation set up. The rayleighs equation was
verified. Relative volatility was determined to be:
.

Relative volatility,

ln ( F / W )
(Graph)

(Eqn)

Mixture I

16

PACKED COLUMN DISTILLATION

Expt:
Date:

AIM:
To find the height equivalent of a theoretical plate (HETP) of packed column at total reflux
for a binary system of A and B by using Fenskes equation and McCabe- Thiele method.
THEORY:

Packed columns are often used for distillation, liquid-liquid extraction , gas absorption and
humidification. For distillation, the gas phase is continuous and the liquid flows in rivulets over the
packing. A packed tower can be used for either continuous or batch distillation.
The design of a distillation tower of the tray column type involves computation of number
of theoretical plates by means of variety of techniques. From this, the total height of the tower can
be calculated. This concept can be adopted for designing packed column also by employing the
term HETP, height equivalent of a theoretical plate. This multiplied by the number of theoretical
plates, calculated from McCabe-Thiele method, gives the total height of packing.
The HETP must be an experimentally determined quantity, characteristic for each type of
packing. It is found that the HETP varies not only with the type and size of packing, but also with
flow rates of each fluid and their composition. The smaller packing has a lower value of HETP.
However it has lower capacity and hence cannot be used in large columns.
The pressure drop per equivalent theoretical plate is generally less than that for a sieve or bubble
cap tray, which is an important advantage for vacuum operation.
Packed distillation columns can be operated over a moderate range of flow rates at nearly
constant separation efficiency. As the capacity parameter increases, both the liquid rate and vapor
rate increase because of which HETP is nearly constant. Structured sheet metal packing gives
slightly better separation than damped packing and the HETP values are nearly constant over a
three to four fold range of flow rates. The more efficient ate the gauze type packing. The gauze is
completely wetted even at low flow rates and the HETP can be predicted from the fundamental
equations of mass transfer in wetted channels. Low surface tension tends to increase the wetted
area, but too low values lead to foaming which increases HETP.

17

PROCEDURE:
1. For distilling the given binary system, known volumes of A and B were mixed and taken in
the distillation flask.
2. Distillation was started. At total reflux, when the top and bottom temperatures reached
constant values, they were noted and the distillate was collected.
3. The residue was cooled. Volumes of the distillate and residue were measured.
4. The density of the distillate and the residue were found.
5. A calibration chart was made by taking a set of mixtures of A and B of varying volume
fractions of A and finding their density. The volume fractions were converted to mole
fractions of A and a graph of mole fraction of A versus density was plotted. This was the
required calibration chart.
6. From the density, the mole fraction of A was found for the distillate and the residue from
the calibration chart.
Observations & Calculations:
Room temperature :
Feed =

ml of A +
Component
A:
B:

ml of B
Density, g / cc Molecular weight, Kg / Kmole

Mole fraction of A:
For a mixture of VA ml of A + VB ml of B:
Moles of A = nA = Mass of A / Mol.wt of A
Moles of B = nB

= (A x VA) / MWA
= Mass of B / Mol.wt of B

where = density
MW = mol. wt

= (B x VB) / MWB
nA
Mole fraction of A, xA = ------------nA + nB

18

Density vs Mole fraction Calibration:

Mixture

I
II
III
IV
V
VI

Volume, ml
A
B

10
8
6
4
2
0

Density,
Mass, g
Sp.gr.
10
ml g/cc
bottle + Sample
sample

Empty
sp.gr
bottle

0
2
4
6
8
10

Mole
fraction
of A, xA
0

Volume, ml

Density, g/cc

Feed
Distillate
Residue

Molefraction of A Temperature, 0 c
xF =
xD =
xW =

Number of theoretical plates:

(i) Fenskes Equation :
xD
( 1 xW )
--------------. -------------( 1 xD )
xW
Nm+ 1 = -----------------------------------Log av
Relative volatility, :
Temperature, 0 c

Vapor pressure, mm Hg
A
B

Rel. volatility,
Vap.pr A
= -----------Vap.pr B

Top
(distillate)
Bottom
(residue)
Average relative volatility, av =

AB =

Nm + 1 =

19

No. of theoretical plates:

Nm

Packing height = Z =

Z
HETP = ---------- =
Nm

(ii) McCabe Thiele Method:

Graph: xA vs yA
Equilibrium Data:
xA
yA
No. of theoretical plates:
=
Nm
Packing height = Z =
Z
HETP = ---------- =
Nm

m
m

RESULT:
An experiment was conducted on the packed column distillation apparatus. The following
results were obtained:
No
1
2

Fenskes
equation
Number
plates
HETP

of

McCabe-Thiele
method

theoretical

20

STEAM DISTILLATION
Expt:
Date:

AIM

To verify the principle of immiscible liquid mixture boiling and finding the vaporization
and thermal efficiencies
THEORY

Steam distillation is a special type of distillation for temperature sensitive materials like
natural aromatic compounds.
Many complex organic compounds
tend to decompose at
high sustained
temperatures. Separation by normal distillation would then not be an option, so water or steam is
introduced into the distillation apparatus. By adding water or steam the boiling points of the
compounds are depressed, allowing them to evaporate at lower temperatures, preferably below the
temperatures at which the deterioration of the material becomes appreciable. If the substances to be
distilled are very sensitive to heat, steam distillation can also be combined with vacuum
distillation. After distillation the vapors are condensed as usual, usually yielding a two-phase
system of water and the organic compounds, allowing for simple separation.
Steam distillation is employed in the manufacture of essential, for instance, perfumes. It is
employed in the synthetic procedures of complex organic compounds. Eucalyptus oil and orange
oil are obtained by this method in industrial scale.
Steam distillation is also widely used in petroleum refineries and petrochemical plants where it
is commonly referred to as "steam stripping". It is used in the food industry for removal of volatile
impurities and flavors from edible fats and oils.
In this experiment, steam distillation is used to separate high-boiling component from small
amount of non-volatile impurities.
When two components A and B which are immiscible exert their own vapor pressure and when
the sum equals total pressure of the system mixture begins to boil. By steam distillation as long as
liquid water is present component A vaporizes at a temperature well below its normal boiling point
without using vacuum. The vapours of the high boiling liquid and water are condensed and the 2
immiscible phases should be separated.
The mole fraction of either of the components in the vapor phase will be proportional to its vapour
pressure. Therefore, the amount of water distilled along with the given immiscible liquid (A) can
be calculated from the relationship,

21

WB=WA x PBMB
PAMA
where WA and WB are weights of component A and water in vapor phase, Kg
PA and PB are vapor pressures of component A and water at distillation
temperature, atm
MA and MB molecular weights of A and water, Kg mole
PROCEDURE
1.
2.
3.
4.

The boiler was filled with water till the drain cock level.
The steam boiler was switched on.
250 ml of nitrobenzene was taken in the still.
The condenser was connected to the still and the water allowed to flow through the
condenser.
5. The steam outlet valve was slightly opened. Care was taken to ensure that steam did not
come out of the condenser.
6. The pressure of steam was maintained at a constant throughout the experiment.
7. The temperature inside the flask rose and at a particular temperature remained a
constant; this temperature was noted as the boiling point of the mixture.
8. The condensate was collected in a conical flask.
9. After the operation the residue was collected in a separating funnel.
10. The distillate was transferred into a separating funnel and was allowed to settle into two
phases.
11. The two phases of residue and distillate were separated and their volumes measured and
noted.
Observations:
Volume of the feed:
cc
Temperature of the feed, TF
=
Temperature of the distillate, TD =

0
0

c + 273 =
c + 273 =

K
K

Density calculation:
Mass,g
Empty sp.gr.
bottle, w
Sp. gr. Bottle +
Substance, wS
Sp. Gr. Bottle +
Water, wW
Sp. Gravity,
wS w
-------wW-w

Distillate
Organic sample Water

Residue
Organic sample Water

22

Mass calculation:
Volume, cc
Distillate

Density, g/cc

Mass, g

Organic sample
Water
Organic sample
Water

Residue

Calculations:
( WA / WB ) Actual
(I) Vaporization efficiency, EV = -------------------------- x 100
( WA / WB ) Ideal
( WA / WB ) Actual

(volume x density) of org. sample in distillate

= -----------------------------------------------------------(volume x density ) of water in distillate

( WA / WB ) Ideal

PAMA
= -----------PB MB

Heat utilized
(II) Thermal efficiency , ET = -------------------------- x 100
Heat supplied

Heat supplied = Steam used [ w + CPw (373 TF) ]

where w = latent heat of steam at 373 K =
CPw = Sp. heat of water =
J / Kg K

J / Kg

=
=

Heat utilized = Mass of org. sample in distillate [sample at TD + Cp sample ( TD TF)]

sample at TD = sample at TB [ (1- TrD) / (1- TrB)] 0.38
where TrD = reduced temperature of distillate

=TD / TC

TrB = reduced normal boiling point of A = TB / TC

TC = critical point of A =
TB = normal boiling point of A =

K
K

23

Cp sample = Sp. heat of sample

sample = latent heat of sample
sample at TD =
Heat utilized =

Thermal efficiency, ET =

(III) Determination of molecular weight:

From the formula

WB=WA x PBMB
PAMA

Molecular weight of the organic sample, MA =

WA x PBMB
----------------

WB x PA
where WA and WB are weights of component A and water in vapor phase, Kg
PA and PB are vapor pressures of component A and water at distillation
temperature, atm

MA and MB molecular weights of A and water, Kg mole

WA =
Kg
Kg
WB =
PA =
atm
PB =
atm
MB = 18 Kg / kmol
MA =

Kg / Kmol

RESULT
An experiment was conducted to verify the principle of immiscible liquid mixture boiling and the
vaporization and thermal efficiencies were calculated.

24

LIQUID LIQUID EQUILIBRIUM

Expt:
Date:
AIM:
To determine the liquid-liquid equilibrium for ternary system- Benzene- Acetic Acid-water.
APPARATUS:
Conical flasks, burettes, micro burettes, beakers, pipettes and agitators.
PROCEDURE:
1) Clean and dry the glass ware.
2) Add 25 ml of Water into 5 conical flasks.
3) Add Acetic acid 4, 8,12,16, 20ml of Acetic acid to each of flasks.
4) Agitate all 5 flasks for 30 minutes.
5) Titrate against Benzene taken in the micro-burette.
6) Take 25ml of benzene in 5 conical flasks.
7) Add 4, 8, 12, 16, 20ml of Acetic acid.
8) Agitate all 5 flasks for 30 minutes.
9) Titrate against Water taken in the micro- burette.
10) Turbidity is the end point for both the cases.
OBSERVATION & CALCULATION:
Density of Acetic acid

_________________

Density of Water

_________________

Density of Benzene

_________________

TABULATION :
Vol of Acetic
acid (ml)
4

Vol of benzene
(ml)

Wt frn of
Acetic acid

Wt frn of
Benzene

Wt frn of water

8
12
16
20

25

Vol of Benzene
(ml)
4

Vol of Acetic
acid (ml)

Wt frn of water

Wt frn of
Acetic acid

Wt frn of
benzene

8
12
16
20

Weight fraction of Benzene = wt of Benzene /(wt.of water + wt.of Benzene)

RESULT: Graph is plotted for the ternary system.

26

SOLID LIQUID EXTRACTION (LEACHING)

EXPT:
DATE:
AIM: To determine the percentage recovery of NaOH by leaching operation.
THEORY:

Mass transfer form solids to liquids with its consequent concentration gradients on a multi
directional basis do not lend itself except in the simplest cases to the normal treatment by
unidirectional diffusion transfer.
If a control surface, S, enclosing a volume, V, of solid in a fluid stream can be considered,
and if mass transfer of a component, A, is taking place from the solid by diffusion, there will be a
mass flow GA per unit area at any point on the surface which may be expressed by equation
GA = -DSL grad CA
Where CA is the concentration of A (mass A/ unit vol. of fluid).
Although this method of percolation leaching is, in reality, a complicated unsteady state
operation, a simple treatment can be devised which amounts to adopting a frame of reference,
which moves with mass transfer zone in the fixed bed. With this approach and by experimentally
determining the logarithmic mean concentration driving force and the total mass transfer rate per
unit area in unit time, experimental values could be obtained for the volume mass transfer
coefficient KV = KC aV where aV = interfacial surface area of contact per unit volume of bed.

C C
A2
N A = KV V A1

C
ln A1

C A2

where,
CA1
CA2
V
NA

=
=
=
=

initial concentration solute in bed

final concentration solute in solvent
volume of bed
mass transferred per unit time per unit cross sectional area of bed.

PROCEDURE:

1. A mixture of 50gm of NaOH(C) and 50gm of CaCo3 (B) were taken into a percolation leacher.

27

2. These were placed in the cotton bag and inserted into the percolation leacher.
3. The solvent tank was filled with the chosen solvent and the electric heater was switched on.
4. The thermostat was set at the desired temperature and temperature allowed to attain the desired
level.
5. The pump was switched ON and the solvent was allowed to enter into the percolation leacher
at fairly slow rate
6. The time was taken from the instant that solvent enters the bed of the leacher.
7. A sample of the mixed solute-solvent was taken from the exit of the bed and the sample was
titrated with the 0.1 N HCl solution.
8. Percentage recovery of sodium hydroxide was calculated.

Observations & Calculations:

Time of operation = t =

minutes

Volume collected after t minutes = V =

litres

Standardization of NaOH:
Normality of HCl = N1=
NaOH vs HCl:
Indicator: Phenolphthalein
S.No Volume of
NaOH, ml

Concordant value, V1 =

Burette reading
Initial
Final

Volume of
HCl, ml

ml HCl

Normality of NaOH = V 1N1 / Volume of NaOH =

=

Amount of NaOH present in V litres = N x eq.wt. x V

= 40 x N x V
Wf =
g

28

Weight of NaOH taken initially = Wi =

Weight extracted

= Wf =

% recovery = (Wf / Wi ) x 100 =

Recovery

RESULT:
An experiment was conducted on the leaching apparatus and the percentage recovery of NaOH by
leaching operation was determined to be..

29

30

31

32

33

BATCH EXTRACTION
Date:
Expt:
Aim:
To determine the percentage extraction in a single stage batch extraction and2 stage batch
extraction.
THEORY:
Extraction is an operation by means of which one or more components of liquid or a solid are
transformed to another liquid. In case of liquid liquid extraction, one of the component must be
sufficiently insoluble so that two liquid phase are formed. The phases are then separated to recover
the desired products. Separation of certain compounds of petroleum base components of the oil by
acetone is an example of extraction.
The liquid is added to bring about the extraction is known as the solvent. The solvent takes
up part of the components of the original solution and forms an immiscible layer and the other
layer, over the remaining.
The solvent layer is called the extract and the other layer, composed of the remainder is
termed as raffinate (plus some amount of the solvent).
This operation is used particularly when separation by distillation is difficult due to the
formation of azeotropic mixture, or non-volatility, or in the cases of substance, which are thermally
unstable.
PROCEDURE:
Single Stage Extraction
1) Take 50 ml of feed C Acetic acid & Benzene and add 30ml of water to it and keep it in the
shaker for 10 min.
2) Using a separating funnel, separate the raffinate and the extract phase.
3) Take 10 ml of each layer and titrate it against NaOH and determine its concentration.
4) Find the density of extract and raffinate.
Two Stage Extraction
1) Take 2 reagent bottles and number them as 1 and 2. To the first bottle, add 50ml of feed
and 15ml of water and keep the mixture in shaker for 10 min.
2) Separate the raffinate and extract layers using a separating funnel.
3) Add 15 ml of water to the raffinate layer and keep it in the shaker for 10 min.
4) Separate the raffinate of the extract layers and titrate it against NaOH.
5) Determine the concentration and density and find the % extract.

34

OBSERVATION:

SINGLE STAGE

DOUBLE STAGE

WEIGHT
FEED EXTRACT RAFFINATE FEED

EXTRACT RAFFINATE

EMPTY
BOTTLE(g)
SAMPLE
+BOTTLE (g)
SAMPLE
TAKEN (g)
VOL.OF
SAMPLE
TAKEN (ml)
DENSITY

Volume of
oxalic acid

Burette Reading
Initial

Volume of
NaOH (ml)

Con.Cordant
Value

Final

35

Estimation of Concentration of solution

S.NO

Volume
of feed
solution
(ml)

Burette Reading

Initial

Volume of
NaOH(ml)

Con.Condant
Value

Final

Estimation of Concentration of Extract:

S.NO

Volume
of Extract
(ml)

Burette Readings

Initial

Volume of Con.Condant
NaOH(ml) Value

Final

36

Estimation of Concentration of Raffinate:

S.NO

Volume of Burette Readings

Raffinate
(ml)
Initial
Final

Volume of Con.Condant
NaOH(ml) Value

SECOND STAGE:
S.NO

Volume of Burette Readings

Extract(ml)
Initial
Final

Volume of Con.Condant
NaOH(ml) Value

37

Estimation of concentration of raffinate:

S.NO
Volume of Burette Readings
raffinate
(ml)
Initial
Final

Volume of Con.Condant
NaOH(ml) Value

Result:
S.NO
1.
2.

NO.OF STAGES

% EXTRACTION

38

Expt:
Date:
TRAY DRYER
AIM:
To find the rate of drying for given material.
THEORY:
Drying a solid means the removal of relatively small amounts of water or other liquid from the
solid material to reduce the content of residual liquid to an acceptable low value. Drying is usually
the final step in series of operations, and the product from a dryer is often ready for final
packaging.
Water or other liquids may be removed from solids mechanically by presses or centrifuges or
thermally by vaporization. This manual is restricted to drying by thermal vaporization. It is
generally cheaper to reduce the liquid content as much as practicable before feeding the material to
a heated dryer.
The liquid content of a dried substance varies from product to product; occasionally the product
contains no liquid and is called bone dry. More commonly, the product does contain some liquid.
Dried table salt, for example, contains about 0.5 % water, dried coal about 4 %, and dried casein
about 8 %. Drying is a relatively term and means merely that there is a reduction in liquid content
from an initial value to some acceptable final value.
The solid to be dried may be in many different forms flakes, granules, crystals, powders, slabs,
or continuous sheet and may have widely differing properties. The liquid to be vaporized may be
on the surface of the solid, as in drying salt crystals; it may be entirely inside the solid, as in
solvent removal from a sheet of polymer; or it may be partly outside and partly inside. The feed to
some dryers is a liquid in which the solid is suspended as particles or is in solution. The dried
product may be able to stand rough handling and a very hot environment or it may require gentle
treatment at low or moderate temperatures. Consequently a multitude of types of dryers are on the
market for commercial drying. They differ chiefly in the way the solids are moved through the
drying zone and in the way heat is transferred.
CLASSIFICATION OF DRYERS:
Drying equipment can be classified according to the following design and operating features:
1. Batch or continuous
2. Physical state of the feed vide liquid slurry andwet solid
3. Method of conveyance of the solid viz belt, rotary, fluidized
4. Heating system: conduction convection, radiation.
EXCEPT

FOR A FEW SPECIALIZED APPLICATIONS, HOT AIR IS USED AS THE HEATING AND MASS

TRANSFER MEDIUM IN INDUSTRIAL DRYERS.

THE

AIR MAY BE DIRECTLY HEATED BY THE

PRODUCTS OF COMBUSTION OF THE FUEL USED (OIL, GAS, OR COAL) OR INDIRECTLY HEATED,

39

USUALLY BY BANKS OF STEAM HEATED FINNED TUBES.

THE HEATED AIR IS USUALLY PROPELLED

THROUGH THE DRYER BY ELECTRICALLY DRIVEN FANS.

Batch dryers are normally used for small scale production and where the drying cycle is likely to
be long. Continuous dryers requires less labor, less floor space; and produce a more uniform
quality product.
When the feed is solids, it is important to present the material to the dryer in a form that will
produce a bed of solids with an open, porous, structure.
For pastes and slurries, some form of pretreatment equipment will normally be needed, such as
extruction or granulation.
The main factors to be considered when selecting a dryer are:
1.
2.
3.
4.
5.
6.
7.

Feed condition: solid, liquid, paste, powder, crystals

Feed concentration, the initial liquid content
Product specification: dryness required, physical form
Throughput required
Heat sensitivity of the product
Nature of the vapor: toxicity, flammability
Nature of the solid: flammability (dust explosion hazard), toxicity.

The basic types used in chemical process industries are: tray, band, rotary, fluidized, pneumatic,
drum and spray dryers.
When wet sample is placed in contact with air, water evaporates from its surface and diffuses as
vapor through the air film that covers the surface. The concentration of moisture at the surface is
decreased, a concentration difference is setup and moisture then diffuses from the interior to the
surface of the slab or it moves to the surface as rapidly as it can vaporize from the surface, the rate
of drying is independent of the moisture content of the slab and is constant providing that the air
velocity, temperature and humidity do not change.
During this constant rate period the rate of drying is controlled by the rate of vapor diffusion
through the air film and is, therefore, dependent upon the humidity difference across the film and
the thickness of the film.
However, when the moisture content becomes less than a certain value known as the critical
moisture content, moisture can no longer move to the surface as rapidly as it could be vaporized
from the surface. The drying rate begins to fall and continues to fall with decreasing moisture
content until the equilibrium moisture content is reached and no further drying is possible under
the particular drying conditions.
During the constant rate period, the rate of drying can be expressed by the following equation.
(1)
dW / d = KgA (pa - pg)
Where,
dW/ d = Rate of diffusion, kg/ hr

40

Kg = Film coefficient of diffusion, kg / hr m2 atmosphere

A = Area of drying surface, m2
pg = Partial pressure of water vapor in the air atmosphere
pa = Partial pressure of saturated air at the water air interface
Since

Y = 18 p / (29 * (1 - p))

Where Y= Humidity kg water / kg dry air

p = Partial Pressure, atm
18, 29 mol. wt. of water and air respectively
Y (18 / 29) p
Then (1) may be written,
dW / d = KgA (Ya Yg)
The drying time during the falling rate period can be calculated from the general diffusion equation
dW / d = - Dg A dC/ dX
Where,
Dg = Diffusivity of water in air
C = Concentration of moisture subject to diffusion in wt. per unit volume
When the experimental drying curve is available, the time required to dry a slab from one moisture
content to another during the falling rate period can be calculated by graphically integrating the
equation
f

W 1 dF
d

=
=f
0
A F2 f ( F )

Where,
f = time of drying, hr
W = weight of dry solid, kg
A = drying area, m2
F1 = free moisture content at the beginning of drying period, kg water/ kg dry solid
F2 = free moisture content at the end of drying period
f(F) = ordinate of the drying rate curve where free moisture content is F kg/ kg dry solid

The total time of during tT, is determined from the following equation:
ms
Xc
tT =
( X 1 X c ) + X c ln

A * Rc
X2
Where,
ms = mass of bone - dry solid
A = area of drying
Rc = rate at first critical point
X = free moisture content, mass of water per unit mass of dry solid

41

Xc = free moisture content at first critical point

X1 = initial free moisture content
X2 = final free moisture content
In deriving the above equation, the entire falling rate period is assumed to be adequately
represented by a singe straight line passing through the origin of the drying curve.
Free moisture content, X, is given by
X = XT = X*
Where,
XT = total free moisture content
X* = equilibrium free moisture content
The equilibrium moisture content of a non porous insoluble material is practically zero so that the
whole moisture content is free moisture.
PROCEDURE:
1. Switch on the power supply to the unit by pressing the ON/OFF key provided on the digital
weighing scale. The scale indicates the weight of the trays and tray cage.
2. Open the drying chamber and take the tray out. Measure the surface area of the trays.
3. Prepare the sample whose drying characteristics are to be determined (here a slurry of
calcium carbonate)
4. Fill the tray with the material and spread it evenly throughout the cross section of the tray.
5. Fill the bulb provided on the back of the tray dryer with water upto topmost level and
provide continuous water (wetting agent) to the wick of wet bulb thermocouples provided
at either ends of the drying chamber.
6. Switch on the blower and adjust the predetermined flow rate of air using the regulator.
7. Switch on the heater. Adjust the temperature of air by using digital temperature controller
provided for the heater on the control panel.
8. After the achievement of a fairly high & stable temperature, note down the decrease in
weight displayed on the digital weighing scale at an interval of 5 minutes. Also note the
wet & dry bulb temperatures of air entering and leaving the drying chamber displayed on
the digital temperature indicator.
9. When there is no loss of weight observed for a prolonged period of time, switch off the
heaters as well as the weighing scale. Take out the trays after they are cooled.
10. Switch off the Blower. Remove the samples from the trays and clean the trays with the
help of cotton cloth first and then with water. Also clean the drying chamber with the
cotton cloth, if there is any spillage of material while operation.
PRECAUTIONS:
1. Never run the equipment without blower ON for more than 1 minute. Switch on the MCB
provided for the heaters only after switching ON the blower.
2. While shutting down the tray dryer, the blower should be kept ON to cool down the drying
chamber and heaters so as to minimize the damage to the heaters and drying chamber.

42

Observations & Calculations:

Drying Chamber Temperature =
Cross sectional Area of the tray =
Total initial weight of the sample =
Density of air
=

Time
min
0
10
20
30
40
50
60
70
80
90
100

Weight
g

Loss of weight
g

c
m2
g
g / cc
Observations
Inlet Air
(DBT) T1 (WBT) T2
0
0
c
c

Outlet Air
(DBT) T3 (WBT) T4
0
0
c
c

43

44

Time
Weight
minutes
g

t
minutes

Calculations
w
g

w / t
g / min

Drying rate
g / hr m2

0
10
20
30
40
50
60
70
80
90
100

45

Graph:
(i) Sample weight in g vs time in minutes
(ii) Drying rate in g /hr m2 vs moisture content,X

dw
NA = ----------Adt
Estimation of Y:
W ( YS Y)
DBT WBT = -------------------------950
where W = latent heat of vaporization at WBT in J / kg
YS = saturation humidity at WBT in kg water vapor / kg dry air
950 ( DBT WBT )
Y = YS -- --------------------------------W
950 ( DBT WBT )
And ( YS Y) = --------------------------W
Estimation of Drying Coefficient, KY:
NA = KY (Ys Y)
KY = NA/(Ys Y)

46

dw
dt

dw
Adt
= NA

DBTAV WBTAV

YS Y

1
YS Y

KY
= dw 1
Adt (YS Y)

g
min

g
m2min

KJ / kg

kg water
kg air

kg air
kg water

g kg air
--------------m2minkg water

47

RESULT:
An experiment was performed on the tray drier and the rate of drying for the given material
(CaCO3) was found to be

48