CH3094 Mass Transfer Laboratory

National Institute of Technology Calicut Department of Chemical Engineering
1. VAPOUR IN AIR DIFFUSION
OBJECTIVE
Study of the effect of temperature on the diffusion coefficient
AIM
To determine the diffusion coefficient of an organic vapour (Acetone) in air
INTRODUCTION
Diffusion is concerned with the movement of individual molecules through a

substance by virtue of their thermal energy. The phenomenon of molecular
diffusion ultimately leads to a completely uniform concentration of substances
throughout a solution which may initially have been non uniform.
So this equipment is very helpful in determining the diffusion coefficient of an
organic vapour. We can also study the effect of temperature on diffusion
coefficient.
THEORY
If two gases are inter-diffusing with continual supply of fresh gas and removal
of the products of diffusion, this diffusion reaches an equilibrium state with
constant concentration gradients. This is known as steady state diffusion. If
also there is no total flow in either direction the rates of diffusion of A and B,
N A and N B are equal but have opposite sign.
According to Daltons law the total concentration of the two components C A
and C B is constant
dC A dC
= B
dx dx
Then using the integrated form of the Ficks Diffusion equation with appropriate
D
NA = (PA1 PA2 ) = N B D (PB1 PB 2 )
RTx RTx
CH 3094 Mass Transfer Laboratory Page 1

1
NOMENCLATURE
C B = Molar concentrations of B, k mole/m3

C T = Total molar concentration, k mole/m3
C BM = Log mean concentration of CH 3 -CO-CH 3 , k mole/m3
D AB = Diffusion coefficient, m2/s
M A = Molecular weight of CH 3 -CO-CH 3 (component A), kg/k mol
P = Total Pressure, k N/m2
R = Gas Law Constant, k N m/k mol K
T = Operating temp, K
VP = Vapour pressure of the evaporating liquid, k N/ m2
x = Final height from top end of the tube after time , cm
x 0 = Initial height from top end of the tube, cm
x 0 x = Drop in liquid (CH 3 -CO-CH 3 ) level in time , cm
= Time of evaporation, sec
l = Density of CH 3 -CO-CH 3 , kg/m3
S = slope of graph sec/cm
AIR (B)
(x0 x )
Acetone
(A)
Fig.1.1 Experimental setup

2
Where P A1 and P A2 are the partial pressures of A at the boundaries of the

zone of diffusion and x is the distance over which diffusion occurs.
C A = Molar concentrations of A, k mole/m3
In case where gas A is diffusing through stagnant gas, B (non-diffusing) the
flow carries both components in proportions to their partial pressure
N A PA N B PB
+
P P
The total transfer of A is the sum of this proportion of the flow and the
transfer by diffusion
PA D dp A
NA = NA
P RT dx
D dp B
N A = N A (1 PB / RT ) +
RT dx
x DP PB 2 dp B
N A dx =
RT PB1 p B
And
0
DP p
NA = ln B 2
RTx p B1
This is the expression used for the experimental determination of vapour

diffusion coefficients in gases by evaporation from a liquid surface in a
narrow bore tube and measuring the fall of level of this surface. The distance of
the liquid surface below the open end of the tube is measured before and after
evaporation over a definite period. If the variation in level is small then
arithmetic mean of these two readings is taken as the value of x . In case there is
appreciable change of level, the value of x is determined by integration
between the initial and final readings of level.
The rate of evaporation is thus given by:

DP p dx
NA = ln B 2 = 1
RTx p B1 M d
Integration of this expression yields:

3
OBSERVATIONS and CALCULATIONS

DATA:
P = ______________ kN/m2
R = ______________ kN.m/kmol.K
l = ______________ kg/m3
MA = ______________kg/kmol
T = ______________ K
OBSERVATION
x0 = _____________ cm
Observation Table:
Sl No. , sec x , cm

4
DP PB 2 M x2
ln
RT PB1

1
0
d = x dx
x1
DP PB 2 M x 22 x12
ln =
RT PB1 1 2
Therefore,
RT l x 22 x12
D=
P
p ln B 2 M 2
PB1
Other form this equation that is convenient to use is:
A [ x 2 x02 ]RTpBM
DAB = (1)
2 P( p A1 p A 2 )M A
In terms of concentration terms the expression for D is:
(x 2
)
x 02 =
2M A D AB C A C T
L C BM
(2)
C B1 C B 2
C BM =
C
ln B1
CB 2
Usually, x 0 will not be measured accurately nor is the effective distance for
diffusion, x, at time . Accurate values of (x x 0 ) are available, however, and
hence:
Rewriting Eq.2 as:
l C BM l C BM
= (x x 0 ) + x0 (3)
x x 0 2 M A D AB C A CT M A D AB C A CT

A graph between against ( x x 0 ) should yield
( x x0 )
l C BM
S= (4)
2 M A D AB C ACT
l C BM
DAB = (5)
2 M AC ACT S
To determine total concentration

5
CALCULATIONS:
(x 0 x ), /(x 0 x )
Sl No.
cm sec/cm
Plot of ( x 0 x) Vs /( x 0 x) from the graph find the slope S
Calculation of vapour pressure, V.P (N/m2) for Acetone at a temperature, T (K)

ln(V .P) = C1 + C 2 / T + C 3 ln T + C 4T C5
Where,
C1 = 69.006
C2 = 5599.6
C3 = 7.0985
C4 = 6.2237 10 6
C5 = 2

6
P
CT = k mol/m3 at operating temperature of K.
RT
Then
(V .P ) A
CA = CT
P
C B1 Shall be equal to CT and
P (V .P ) A
C B 2 = CT , k mol/m3
P
Evaluation of vapour pressure of Acetone (CH 3 -CO-CH 3 )
So Relation between temperature & Vapour pressure from this curve
Effect of temperature and pressure on co-efficient of diffusion, D is expressed as:

D = Const.T1.5/P
D can be determined by drawing a curve of DP Vs. T.
DESCRIPTION
The equipment consists of a T tube made of glass, placed in a constant
temperature water bath. Temperature of the bath is controlled by the DTC. Air
pump is used to supply the air, passed through the T tube. Volatile component is
filled in the T tube and air passed over it by the pump and change in the level is
seen by the sliding microscope.
PROCEDURE
1. Clean the apparatus and make it free from dust.
2. Fill 3/4th water bath with water.
3. Set the water bath temperature at the desired level (up to 50 C) and wait
till the bath attains the set temperature. Note the steady temperature of the
bath.
4. Fill the T-tube with Acetone (CH 3 -CO-CH 3 ) up to within two centimetres
of the top of capillary leg. Note down the initial diffusion height of liquid
in the capillary.

7
P
CT = , kmol / m 3 =
RT
= k mol/m3
VP
C A = CT , kmol / m 3 =
P
= k mol/m3
From Graph, S = sec/cm2 = 10-4 sec/m2
C B1 = CT , kmol / m 3 = k mol/m3
( P VP)
C B 2 = C B1 , kmol / m 3 =
P
= k mol/m3
C B1 C B 2
C BM = , kmol / m 3 =
C B1
ln
CB 2
= k mol/m3
l C BM
DAB = , m 2 / sec =
2 M AC ACT S
= m2/sec

8
5. Make the connection with the Air or vacuum pump and allow a gentle
current of air to flow over the capillary.
6. Record the height of liquid (x) in the capillary after every__________ min
7. Repeat the steps 1 through 5 for different water bath temperatures.
8. Use different organic liquids like: ethanol, toluene, CCl 4 , hexane etc. and
tabulate the results and discuss.
RESULTS
INFERENCE

9
2. WATER COOLING TOWER
OBJECTIVE
To study the heat & mass transfer operation in Water Cooling Tower for
different flow & thermodynamic conditions.
AIM
To determine the overall heat transfer coefficient in a forced draft counter
current cooling tower.
KaV
To measure Tower Characteristic parameter for various liquid and air flow
L
L
rates in a counter-current Forced draft Cooling Tower.
G
INTRODUCTION
Water from condensers and heat exchangers is usually cooled by an air stream in
spray ponds or in Cooling Towers using natural draft or forced flow of the air.
Mechanical draft towers are of the forced draft type, where the air 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 as long as its temperature is above the wet bulb
temperature of the entering air. Markels theory is used which is based on enthalpy
potential difference as the driving force.
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.
10
Air out (G2, T3, T4, H1) Water in (L1, T5)
Packing
Cooling
Tower
Air in (G1, T1, T2, H2) Water out (L2, T6)

Fig.2.1 Schematic representation of a vertical counter current cooling tower
Fig.2.2 Counter flow Cooling Diagram
11
Then the enthalpy balance is.

GdH G = LdH L (1)
(Where H L & H G are the enthalpies of liquid and gas phase respectively)
The rate of heat transfer from liquid to interface is

QL = LH L = hL (TL Ti ) AdZ (2)
The rate of heat transfer from interface to gas is

QG = GH G = hG (Ti TG ) AdZ (3)
Where hG & hL = heat transfer coefficient
A = heat transfer area

Z =height of the tower
Ti = interface temperature
Then, the rate of heat transfer from interface to gas
GCG (TG1 TG 2 ) = GdH G = hG (Ti TG ) AdZ (4)
These above equation can be simplified and rearranged to find out the heat transfer
coefficient.
The enthalpy of the liquid

H L = C L (TL TO ) (5)
Where C L = specific heat of liquid
TO = base temperature for computing enthalpy

Then,
LdH L = LC L dTL (6)
Putting it in Equation (2)
We will get,
LC L dTL = hL (TL Ti ) AdZ (7)
So, equation for liquid phase heat transfer,

dTL h AdZ
= L (8)
TL Ti LC L
12
OBSERVATION AND CALCULATION:

DATA:
d1 = _____________ m
d 2 = _____________ m
C d = _____________
w = _____________ kg / m 3
a = _____________ kg / m 3
g = 9.81 m / s 2
OBSERVATION TABLE:
Sl T1 , C T2 , C T3 , C T4 , C T5 , C T6 , C R1 , cm , R2 , cm Qw
No. LPH
13
Then, for gas phase heat transfer,

dTG h AdZ
= G (9)
Ti TG GCG
The total amount of heat transferred,
Q = UAZ (T )
Where U = overall heat transfer coefficient
At steady state Q = QG = QL
So,
hL hG
U= (10)
hL + hG
For mass transfer operation:
Each particle of water is assumed to be surrounded by a film of air and the enthalpy
difference between the film and the surrounding air provides the driving force for the
cooling process. In the integrated form Markels equation can be written as:
KaV T5 dT
= '
L T6 h h
Tower characteristic can be evaluated numerically by :
KaV T5 dT T T 1 1 1 1
= = 5 6 + + + (11)
L T6 h h
w a 4 h1 h2 h3 h4
Tw1 = T6 + 0.1(T5 T6 )
Tw 2 = T6 + 0.4(T5 T6 )
Tw3 = T5 0.4(T5 T6 )
Tw 4 = T5 0.1(T5 T6 )
ha1 = h1 + 0.1( L / G )(T5 T6 )

ha 2 = h1 + 0.4( L / G )(T5 T6 )
ha 3 = h2 0.4( L / G )(T5 T6 )
ha 4 = h2 0.1( L / G )(T5 T6 )
And hi = hwi hai
14
CALCULATIONS:
OVERALL HEAT TRANSFER COEFFICIENT
R1 R2 w
H = 1 , m of air =
100 a
= ------------------------ m

a1 = d12 , m2 =
4
= _____________________m2

a2 = d 22 , m2 =
4
= _____________________m2
a1a 2
Qa = C d 2 gH , m3/sec =
a a
2
2
2
1
=______________________m3/sec
G = Qa a , kg/sec =
= ____________________kg/sec
Qw w
L= , kg/sec =
1000 3600
=_____________________kg/sec
L
=
G
= _______________
15
The carrying of liquid with the gas stream is termed as Liquid Entrainment. This may
be due to a high rate of air flow. This should be avoided to get better performance.
This can be avoided by following the operational limits of the equipment.
DESCRIPTION
The apparatus is provided for the process of Forced draft counter current cooling of
hot water using air. The water to be cooled is heated in a heating tank using a heater.
It is then circulated; through a rotameter; to the top of the cooling tower mounted
over the heating tank. Cooled water is then re- circulated to the heating tank. A
blower is provided for the cooling air. A valve is provided in 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 gives dry bulb and wet bulb air
temperatures. The cooling tower is packed with Aluminium expanded wire mesh.
UTILITIES REQUIRED
1. Electrical supply: Single Phase, 220 V AC, 50 Hz, 5-15 amp socket with
earth connection.
2. Water Supply
3. Drain required.
4. Bench Area Required: 1.2 m x 1m
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
From Enthalpy table,
16

The enthalpy of entering air at a wet bulb temperature ( T2 , C )
h1 = ha = ________________
Enthalpy of leaving air (h2) is,
h2 = ha = h1 + ( L / G )[T5 T6 ] =
= ________________________
T , F hwi hai hi = hwi hai
T = T6 = hw = ha = h1 =
T = T6 + 0.1(T5 T6 ) hw = ha = h1 + 0.1( L / G )(T5 T6 )
T = T6 + 0.4(T5 T6 ) hw = ha = h1 + 0.4( L / G )(T5 T6 )
T = T5 0.4(T5 T6 ) hw = ha = h2 0.4( L / G )(T5 T6 )
T = T5 0.1(T5 T6 ) hw = ha = h2 0.1( L / G )(T5 T6 )
T = T5 = hw = ha = h2 =
4. Record the flow rate of water and manometer reading after steady state achieved.
17
5. Record the temperatures.

6. Steps 3 to 5 may be repeated for different water & air flow rates
within operational range.
NOMENCLATURE
A = Cross sectional area of column , 2
a1 = Cross section area of Orifice , 2
a2 = Cross section area of pipe , 2
Cd = Coefficient of discharge
CG = Specific heat of gas, kJ/kg C
CL = Specific heat of liquid, kJ/kg C
d1 = Diameter of orifice, m
d2 = Diameter of pipe, m
Qw = Flow rate of water, LPH
g = Acceleration due to gravity, m/ 2
G = Mass velocity of air, kg/s 2
H = Head loss, m
hG = Heat transfer coefficient (interface to gas phase), W/2 C
hL = Heat transfer coefficient (liquid to interface), W/2 C
h1, h2 =Enthalpy of air at wet bulb temperature, btu/lb of dry air
hw = Enthalpy of water, btu/lb of dry air
ha = Enthalpy of air, btu/lb of dry air
K = Mass transfer coefficient, lb water/ 2 sec
L = Mass velocity of water, kg/s 2
Ma = Mass flow rate of air, kg/sec
Mw = Mass flow rate of water, kg/sec
Qw = Flow rate of water, 3 /sec
Qa = Flow rate of air, 3 /sec
KaV
Tower characteristic, =
L
18
Knowing V and L the mass transfer coefficient Ka can be calculated Determine [Ka
V /L] for various values of L/G and plot the values. Cooling range = T5 T6 =
Temperature approach = T2 T6 =
Mass transfer coefficient

T5 , C = _______________ C = ________________ F
T6 , C = _______________ C = ________________ F
Tw1 = T6 + 0.1(T5 T6 ) =
hw1 = btu/lb of dry air
Tw 2 = T6 + 0.4(T5 T6 ) =
hw 2 = btu/lb of dry air
Tw3 = T5 0.4(T5 T6 ) =
hw3 = btu/lb of dry air
Tw 4 = T5 0.1(T5 T6 ) =
hw 4 = btu/lb of dry air
At T4 C (Leaving air wet bulb temperature)

h1 = ------------------------btu/lb of air
h2 = h1 + ( L / G )(T5 T6 ) , btu/lb of dry air =
= ______________________btu/lb of dry air
ha1 = h1 + 0.1( L / G )(T5 T6 ) , btu/lb of dry air =
= ______________________btu/lb of dry air
T1 = Air inlet dry-bulb temperature,C
19
T2 = Air inlet wet-bulb temperature,C

T3 = Air outlet dry-bulb temperature,C
T4 = Air outlet wet-bulb temperature,C
T5 = Water inlet temperature,C
T6 = Water outlet temperature,C
Ti = Average interface temperature,C
Ta = Air temperature,C
Tw = Water temperature,C
TG = Temperature of the gas ,C
TL = Temperature of the liquid ,C
U = Overall heat transfer coefficient W/2 C
V = Effective volume of column, 3
Y1, Y2 = Humidity, kg/kg of dry air
Z = Height of packing, m
w = Density of manometer fluid(water), kg/3
a = Density of air, kg/3
PRECAUTIONS
1. Heater should not be switched on before filling the water in heating tank.
2. Pump should not be switched on at low voltage.
3. Water in heating tank should be properly drained after experiment is over.
4. Cotton jacket over the wet bulb arrangement should be in its place properly.
5. Wet bulb bottle should be filled with water before starting the experiment.
RESULTS
ha 2 = h1 + 0.4( L / G )(T5 T6 ) , btu/lb of dry air =
20
= ______________________btu/lb of dry air
ha 3 = h2 0.4( L / G )(T5 T6 ) , btu/lb of dry air =
= ______________________btu/lb of dry air
ha 4 = h2 0.1( L / G )(T5 T6 ) , btu/lb of dry air =
= ______________________btu/lb of dry air
h1 = hw1 ha1 , btu/lb of dry air =

= ______________________btu/lb of dry air
h2 = hw 2 ha 2 , btu/lb of dry air =
= ______________________btu/lb of dry air
h3 = hw3 ha 3 , btu/lb of dry air =
= ______________________btu/lb of dry air
h4 = hw 4 ha 4 , btu/lb of dry air =
= ______________________btu/lb of dry air
1 1 1 1
h + + + =
h2 h3 h4
1
=________________________
KaV T5 dT T T 1 1 1 1
= = 5 6 + + +
L T6 h h
w a 4 h1 h2 h3 h4
21
3. ADSORPTION ISOTHERM
OBJECTIVE
To verify the applicability of the Freundlich equation for adsorption of acetic
acid on activated carbon and to determine the value of constants k and n in equation
for adsorption at room temperature.
APPARATUS
Reagent bottles, conical flasks, filtering funnel, burette, pipette, volumetric flask
CHEMICALS REQUIRED
Acetic acid, activated carbon, 0.1N NaOH solution, Oxalic acid
THEORY
Adsorption isotherm exploits the ability of certain solids preferentially to
concentrate specific substances from solution to their surfaces. In this, components of
either liquid or gaseous solution may be separated from each other. Some applications
of adsorption in gaseous separations are de-humidification of air and other gases,
removal of objectionable odours of impurities from industrial gases, recovery of
valuable solvent vapors from dilute mixtures with air and other gases and
fractionation of mixtures of hydrocarbon gases containing such substances like
methane, ethane and propylene. Typical liquid separation is removal of moisture
dissolved in gasoline, decolourisation of petroleum products and aqueous sugar
solution, removal of objectionable taste and odour from water and fractionation of
mixture of aromatics and paraffinic hydrocarbons.
Adsorption can be physical or chemical. Physical adsorption or Vander
Waals adsorption can be readily reserved and is the result of intermolecular forces of
attraction between solid and the substance adsorbed. The equilibrium partial pressure
of the substance adsorbed equals that of contacting gas phase. This is lower than the
vapour pressure and so adsorption is not simple condensation. By lowering the
22
OBSERVATIONS
Room Temperature = _________ C
Weight of weighing tube =
Weight of weighing tube + acetic acid =
Weight of acetic acid taken in 250ml flask (F1) =
Normality of Oxalic acid =
1. Standardization of 0.1 N NaOH Indicator: Phenolphthalin
Titre value of Oxalic acid (ml)

Sl No.
Vol. of NaOH (ml)
Titre 1 Titre 2
2. Preparation of mixtures
Vol. taken Vol. of Wt. of paper Wt. of paper Wt. of
from F 1 to solution + Carbon + Carbon Carbon
250 ml transferred before after taken
Bottle No.
flask, F 2 to bottle transferring transferring (g)
(ml) from F 2 (g) (g)
(ml)
B1
B2
B3
B4
B5
23
pressure of gas phase by raising the temperature, the adsorbate is readily removed or
desorbed in unchanged form, reversible adsorption is seen in liquids as well.
Chemisorption or activated adsorption is the result of chemical interaction between
the solid and the adsorbed substance. The process is frequently irreversible and on
adsorption, the original substance will be found to have undergone a chemical
change. Chemisorption finds applications in catalysis. The usual adsorbents are
fullers earth, activated clays, bauxite, alumina, bone charcoal, decolourising carbon,
gas adsorbent carbon, silica gel, zeolites and metal alumino-silicates.
Adsorption equilibria
The amount of substance adsorbed depends on the concentration of the

contacting gas or liquid phase, the temperature and pressure. A relationship among
these variables is called adsorption equilibria. Data on equilibria are essential for
designing adsorption unit. Equilibrium data expressed for a particular temperature is
called adsorption isotherm.
Saturation vapour pressure
Actual condensation starts

from this point
Equilibri
-um
partial
pressure
of gas, P*
g adsorbed/ g of adsorbent
In liquid adsorption, isotherms are important since no appreciable volume

changes of the liquid occur which might be used as a measure of adsorption.
24
3. Titration of filtered solution Indicator: Phenolphthalin

Volume of
Bottle solution Diluted Volume of Titre value of Acetic
No. used for Volume NaOH acid
dilution (ml) taken (ml)
(ml) (ml) Titre 1 Titre 2
B1
B2
B3
B4
B5
CALCULATIONS
Volume of Oxalic acid (ml ) Normality of Oxalic acid ( N )

Normality of given NaOH solution ( N ) =
Volume of NaOH solution (ml )
The value of V (cm3 of solution/ g of adsorbent) and C 0 in each of the five bottles are
calculated. The value of C in each of the original filtered solution is found out by
N NaOH V NaOH Equivalent weight of Acetic acid

C =
Volume of Acetic acid 1000
25
Withdrawal of the solid and weighing it, as can be done in the case of gases, will not
distinguish between the adsorbed liquid and that which is mechanically occluded.
When adsorbent is mixed with a binary solution, adsorption in both solute and solvent
occurs. Since the total adsorption cannot be measured, the relative or apparent
adsorption can be determined instead. The customary procedure is to treat a known
volume of solution with a known weight of adsorbent. V cm3 of solution/gm of
adsorbent. As a result of preferential adsorption of solute, the solute concentration of
the solution is observed to fall from initial c 0 to final C* in the liquid(c-concentration
expressed in g of solute per cm3 of solution). The apparent adsorption of solute,
neglecting any adsorption of solvent is V(C 0 -C*) g of solute adsorbed per gram of
adsorbent. This is satisfactory for dilute solutions where the fraction of the original
solvent, which may be adsorbed, is small. Particularly for dilute solutions, the
adsorption isotherm may be described by an empirical expression,
C * = k [V (C 0 C *]
n
(1)
Where, k and n are constants at particular temperature. It is to be noted that n is

independent of units used and k has units same as that used for C or C0 .
Sometimes this curve may show deviation from linearity. This may be due to
appreciable adsorption of the solvent or simply the general inapplicability of the
Freundlich expression.
PROCEDURE
Record the room temperature. Weigh about 25 g of Acetic acid exactly in
weighing bottle and transfer it completely by repeated washings to a 250 ml
volumetric flask (F 1 ) and make up the volume with distilled water. Pipette out 10 ml
of this solution into another 250 ml volumetric flask (F 2 ) and the volume is made up.
Weigh about 5 g of activated carbon into a reagent bottle (B 1 ) by differential
weighing. Add 200 ml of solution from flask (F 2 )
26
For bottle, B 1
200
Volume of solution /g of adsorbent (V) = = 40 cm3/g
5
Initial concentration of solution,
(25 10) / 250
C0 = = 4 10 3 g solution / cm 3 of solution
250
Generally,
Weight ofAceticacid ( g ) Volume taken (ml )
C0 =
Diluted volume (ml ) Total diluted volume (ml )
=
V(C 0 C*) =
lnV(C 0 C*) =
27
to this bottle. Repeat the same procedure with bottle numbers B 2 , B 3, B 4 , B 5 with the
difference that the volumes of solution pipette out from the flask F 1 are 20 ml, 30 ml,
40 ml and 50 ml respectively. Shake the bottles well for one hour using bottle shaker
for adsorption to come into equilibrium. Mean while prepare a standard solution of
Oxalic acid (0.1 N) and use this to standardize the supplied NaOH solution. After 1 hr
shaking, filter the solution and titrate in the five bottles. Take the solutions in the
burette and titrate it against 10 ml NaOH.
RESULT
INFERENCE
28
Bottle V C0 C*
No. (cm3 of (g of solute/ ml (g of solute/
V(C 0 C* ) ln C* ln [V(C 0 C* )]
solution/ g solution) ml solution)
adsorbent)
B1
B2
B3
B4
B5
29
4. SIMPLE LEACHING
OBJECTIVE
1. To draw the percentage actual recovery against solvent to feed ratio for single stage
leaching. Also, to compare actual recovery with the theoretical recovery.
2. To draw the percentage actual recovery Vs the number of stages curve keeping the
solvent to feed ratio constant and to compare the actual recovery with the theoretical
recovery.
APPARATUS
1. 500 cc beakers (6 No)
2. Pipettes - 500 cc (1), 20 cc (1 No), 5 cc (1 No)
3. Burette (50 cc)
4. Volumetric Flask (100 cc)
5. Conical Flask (250 cc)
CHEMICALS
1. Sand
2. Sodium Carbonate
3. N/10 HCl Solution
30
OBSERVATIONS
VARYING SOLVENT TO FEED RATIO
Solvent used
Beaker Sodium in extraction Solvent to
No. Carbonate(gm) Sand(gm) Water(ml) (ml) feed ratio
STRENGTH OF EXTRACT INDICATOR: METHYL ORANGE
Extract used Volume taken Titre value of HCl (ml)

Beaker Makeup
for dilution for dilution
No. volume (ml)
(ml) (ml) Titre value 1 Titre value 2
31
THEORY
The methods of removing one constituent from a solid or liquid mixture by a
liquid solvent fall into two categories. If the soluble matter is dissolved from its
mixture by an insoluble solid, the operation is called leaching or solid extraction. The
second, called liquid extraction is used to separate two miscible liquids by the use of a
solvent.
The following are some terms connected with leaching. The mixture of the
insoluble carrier solid plus the solute which is to be separated is called the feed. The
feed is contacted with the solvent and the mixture is separated into two streams. The
solvent rich product of the operation is called the extract or the overflow and the
stream that contains the bulk of the carrier solid is called the leached solids or
underflow. A unit of equipment in which the above mentioned operation is carried out
is called a stage. In simple batch leaching operation, if sufficient amount of solvent is
used, all the solute can ultimately be dissolved in the solvent. The amount of solute
that comes out with the extract based on this assumption is called the theoretical
recovery. But actual recovery will be less than the theoretical recovery because
The solute may be incompletely dissolved because of inadequate contact time
and
The solids leaving the stage retain some of the solute.
The method of operation of leaching can be classified into
1. Batch wise (unsteady State)
2. Continuous (steady State)
Here, in this experiment, we study the principles of batch leaching.
32
VARYING NUMBER OF STAGES
Sodium Extract Total amount of

Beaker Sand Water Number
carbonate per solvent used for
No (gm) (ml) of stages
(gm) stage(ml) extraction (ml)
STRENGTH OF EXTRACT INDICATOR: METHYL ORANGE
Extract used Made up Volume taken

Titre value of HCl (ml)
Beaker No. for dilution volume (ml) for
(ml) titration(ml) Titre 1 Titre 2
STANDARDISATION OF HCl (Indicator: Methyl Orange)

Weight of Na 2 CO 3 =
Made up volume of Na 2 CO 3 solution =
33
PROCEDURE
1. Varying solvent to feed ratio

Prepare a 10% by weight mixture of sodium carbonate and sand by accurately
weighing about 45g of sand and 5 g of sodium carbonate. Add 50 cc of distilled water
to this mixture. This is the feed.
Prepare five different feed sample in 500 cc beaker. Now, add an additional
50 cc of distilled water to beaker. Stir the mixture well and allow the sand to settle for
a few minutes. Now pipette out 50cc of clear solution from this beaker into a clean
empty beaker. To bring down the normality of the extract to approximately that of
HCl the following procedure is suggested. Pipette out 10cc of extract and make up the
volume to 100cc. Using a volumetric flask, transfer 20cc of this solution to a conical
flask and titrate against HCl taken in the burette. Note that the solvent to feed ratio by
volume used in the above experiment is on sand (unit) free basis.
Repeat the procedure with feed taken in beakers 2,3,4 and 5 with the
following difference. To beaker 2, add 1000cc of water to a clean beaker. That is,
feed in beaker 2 is extracted with 150cc, 200cc and 250cc of solvent respectively. In
each case, do suitable dilution of extract before it is titrated against HCl taken in the
burette.
2. Varying number of stages

Prepare a 10% by weight mixture of sodium carbonate and sand by accurately
weighing about 45g of sand and 5g of sodium carbonate. Add 50cc of distilled water
to this mixture. This is feed. Prepare the feed in 5 beakers. Extract the solute from
each beaker with 200cc of water but vary number of stages from 1 to5. This is done
as follows. To beaker 1, add 200cc of water, stir the contents well, allow the sand to
settle and pipette out 200cc of clear solution. Titrate it against HCl to beaker 2, add
100cc of water and pipette out 100cc of clear solution into a clean beaker. Now, add
100cc of fresh water again to the slurry and after mixing well, pipette out 100cc of
34
Titre value of HCl (ml)
Volume of
Na 2 CO 3 solution Titre 1 Titre 2 Titre 3
(ml)
CALCULATIONS
Normality of standard Na 2 CO 3 solution + HCl solution are determined
Weight of Na 2 CO 3 , W 1 =
Equivalent weight of Na 2 CO 3 , M 1 =
Normality of Na 2 CO 3 , N 1 = (W 1 /M 1 ) =
Normality of HCl, N 2 = (V 1 N 1 ) / V 2 =
1. Varying solvent to feed ratio:

The normality of extract in each case is found out
Normality of makeup solution = (V HCL N HCL ) / V EXTRACT =
Normality of extract =
35
clear solution and mix it with the earlier extract. Find strength of this combined
extract by titrating against 0.1 N HCl solution.
Beaker 3: Extracted 3 times using 66.6cc of water each time.
Beaker 4: Use 50cc of water four times.
Beaker 5: Use 40cc of water five times.
A standard solution of sodium carbonate approximately 0.1 N is prepared and
this is used to standardize the HCl needed.
36
Solute extracted = (N EXTRACT Eq weight of Na 2 CO 3 volume of extract) / 1000
Vol. of extract
Theoretical % recovery = 100
Vol. of liquid when feed and solvent are mixed
% actual recovery = (Solute extracted 100) / Na 2 CO 3 taken
Calculation of theoretical recovery for varying number of stages.
% theoretical recovery = (volume of extract 100) / (Volume of liquid when feed

+Solvent are used)
=
Normality of Solute % actual % theoretical

Mixture no extract extracted(gm) recovery recovery
In the graph theoretical & actual % recovery are plotted on the y axis against the
solvent to feed ratio taken in the x axis.
37
RESULT
1) Percentage theoretical recovery and actual recovery is plotted against solvent to feed
ratio. Also the graph for theoretical and actual recovery Vs number of stages is
plotted.
2) Both these graphs conclude that leaching increases with the amount of solvent used
and also with number of stages.
3) Theoretical recovery was found to exceed actual recovery and it increased with the
number of stages.
INFERENCE
38
2. Varying Number of Stages:

The normality of extract at each case is found as
Normality of make-up solution, N =
Normality of extract, N =
R 1 = (E 1 /V 1 )100 =
R 2 = (100-R 1 )(E 2 /V 1 ) =
Rn= (100-R n-1 )(E n /V n ) =
Overall theoretical % recovery = (R 1 +R 2 ) = %
Normality of Solute % actual % theoretical

Beaker No extract extracted(gm) recovery recovery
In the graph the theoretical and actual % recoveries are plotted against number of
stages.
39
5. COUNTER CURRENT LEACHING
OBJECTIVE
To find the overall efficiency of a counter current leaching unit by batch
simulation of a conter cascade.
APPARATUS
1. 500 cc beakers (5 no.s)
2. Burette
3. Pipettes(50 cc,20 cc,5 cc)
4. Volumetric flask(100 cc,250 cc,500 cc)
5. Conical flask(250 cc)(2 no.s)
6. Funnel
CHEMICALS
1. Sand
2. Sodium Carbonate
3. HCl (approx.. 0.1 N)
THEORY
The operation of leaching has been explained in the experiment on simple
leaching. The meanings of the terms feed, extract leached solids and recovery as
applied to leaching are also explained there. Leaching can be done either batch
wise on continuously. When continuous steady state leaching is done by stage
wise contacting, counter current multistage leaching is the most common method
of operation .In this the solids to be leached and the solvent move in the opposite
directions. That is the leached solids from the first stage is fed to the second stage
as feed, the leached solids from the second stage is fed to the third stage as feed
etc, while the extract from the nth stage is used as the solvent for (n-1)th stage, the
extract from the (n-1)th stage is used as solvent for the (n-2)nd stage and so on.
The method of finding the number of stages required to reduce the solute
content of the solids to some specified value using the equilibrium stage
approach has been explained.
40
Counter current cascade arrangement
50 ml Feed
200 ml Soln discarded B1 200 ml H2O

50 ml Feed
200 ml
n
200 ml Sol discarded B2 B1 200 ml H2O
50 ml Feed
200 ml 200 ml
n
200 ml Sol discarded B3 B2 B1 200 ml H2O
Figure 1
50 ml Feed
200 ml Soln to conical 200 ml 200 ml
flask B4 B3 B2 200 ml H2O
Figure 2
200 ml Soln discarded B3 200 ml H2O
200 ml Soln discarded 200 ml

B4 B3 200 ml H2O
50 ml Feed
200 ml 200 ml
B5 B4 B3 200 ml H2O
200 ml Soln to conical

flask Figure 3
41
So the definition of overall stage efficiency, notation scheme and the graphical
representation is same as of the number of stages.
PROCEDURE
Weigh about 50 g of Na 2 CO 3 and transfer it to a 500 cc volumetric flask
and the volume is made up with distilled water. The beakers are marked B1, B2,
B3, B4 and B5. Weigh about 10 g of sand into each of the different beakers. To
each beaker, add 50 cc of prepared solution using a pipette, which is known as
Feed. The method of batch simulation of the counter current cascade is as follows.
Add 200 cc water into beaker B1 and after stirring well, allow sand to settle,
pipette out 200 cc of clear solution and discard it. Now extract the contents of this
beaker using 200 cc water and transfer the 200 cc to beaker B2 using a pipette
after stirring well, allow sand to settle. Discard 200 cc of the clear solution from
this beaker (B2). This is continued till all operations of Fig.2 are completed.
The 200 cc of extract from B4 is transferred to a clean dry conical flask
and the solution is filtered into another dry conical flask. By this stage, steady
state operation might have attained. For this 50 cc of the solution obtained in the
conical flask as extracted from B4 is pipetted into a 250 cc Volumetric flask and
the volume is made up with distilled water. 20 cc of this solution is taken in a
clean conical flask and titrated against 0.1 N HCl taken in a burette. Now the
leaching process is continued as shown in figure 3.
The solution obtained as extract from B5 is filtered, diluted and titrated
against 0.1 N HCl as described in the previous paragraph. If the titre value is the
same as obtained earlier, steady state counter current operation has been attained.
The solution of the leached solids from B3 is filtered into a clean conical flask ,
40 ml of this solution is titrated against the HCl taken in the burette. A standard
solution of 0.1 N Na 2 CO 3 is prepared and this is used to standardize the HCl
solution used.
42
OBSERVATION
Beaker Volume of Volume of Volume of Titration value
number extract used diluted extract solution for (ml)
for dilution (ml) titration(ml) Titre 1 Titre 2 Titre 3
(ml)
B4
B5
B3
CALCULATION
C=AY
1-Y
N=
10/(50 + C)
A rectangular coordinate system with N on Y-axis and x, y on X-axis is used for
the graphical calculation. While calculating the ideal stages, we proceed with
assumption that NO INERT IS TAKEN away with the extract. So any point
denoting the composition of an extract has to be on X-axis. This is the locus of
OVER FLOW. Similarly the points denoting all leached solids composition fall on
a curve, which is called the locus of UNDER FLOW. We take different y values
and for each one of these calculate N using the following equations.
43
RESULT
The fractional efficiency of the leaching process is ________.
Fractional stages required is ________.
INFERENCE
44
A = 50 gm
C = A[y/(1-y)]
Let, y = 0.01
C = 50[0.01/(1-0.01)] = 0.505
N = B/(A+C)
B is the weight of sand in each stage
= 10/(50+0.505) = 0.198
Weight of Na 2 CO 3 taken in 50 ml flask, gm =

Weight of sand taken in each beaker, gm =
Normality of standard Na 2 CO 3 solution = N
Normality of HCl = (N x V) Na2CO3 /V HCl =
N HCl Titre volume of HCl makeup volume of extract

Normality of Extract =
Volume of so ln taken for titration volume of extract for dilution
= N
Normality of extract 53 200

Weight of extract of Na2CO3 in 200mL extract,C =
1000
= gm
Titre value for leached solids = ml
N HCl Titre value

Normality of the leached solution =
Volume of the solution
45
46
= N
Normalityof So ln 53 50
Wt. of Na2CO3 in 200mL of So ln adhearing to leached So ln =
1000
= gm
y F = grams of Na 2 CO 3 in each feed / (50 + grams of Na 2 CO 3 in each feed)
50
50
= 500 = 0.0909
50
50 + 50
500
y 3 actual = gram of Na2CO3 in leached solids / (50 + Weight of Na 2 CO 3 in 200mL

extract)
=
N 3 actual = gram of sand taken / (50 + gram of Na 2 CO 3 in leached solids)
10
= =
50 + _____
With reference to graph,
Fractional stage required = (y 3 actual -y 2 )/(y 3 -y 2 )
Integral number of stages required = 3
47
48
Fractional ideal stages required = 2+ Fractional stage required =

=
Theoretical no. of stages =

Actual no. of stages =3
Overall efficiency = (Theoretical no. of stages /Actual no. of stages) x 100
49
6. TERNARY LIQUID EQUILLIBRIUM
OBJECTIVE
To draw the binodal solubility curve for the system Glacial acetic acid -Benzene
Water at room temperature and pressure.
APPARATUS
1. 50cc burette (3 no.s)
2. 50cc test tube (10 no.s)
3. Density bottle.
CHEMICALS
1. Glacial acetic acid
2. Distilled water
3. Benzene
THEORY
Consider the liquid extraction operation, where we are interested in separating
acetic acid from a mixture of acetic in water. The liquid is agitated with a liquid such
as ethyl acetate. Some of the acid but relatively less amount of water will enter the
liquid phase. So the difference immiscibility of acetic acid and water in ethyl acetate
and water is taken advantage of in separating the mixture.
In all such operations we see that
1. There are at least three substances and two phase involved.
2. The two liquid phases finally reach equilibrium when they are kept in contact
with each other, for which sufficient length of time. Study the composition of
two phases which are in equilibrium with each other and each of which
involves three components called ternary liquid equilibrium.

50
Fig.6.1. Ternary composition in an equilateral triangle
Fig.6.2 Liquid-Liquid equilibrium data represented in the equilateral triangular

coordinates

51
All possible composition of three substances involved can be divided into two groups:
Compositions in which the ternary system exists as a single phase (three
liquids are completely miscible)
Compositions in which the system exists in two phases .Hence in liquid
extraction design, it is important to determine the following experiments.
The Compositions at which the system changes from a completely miscible in to a

two phase system. If all compositions of ternary liquid system can be represented on a
graph paper. The boundary between miscible and immiscible regions can be
represented by a curve. This curve is called binodal curve.
At a given condition of temperature and pressure, composition of one phase
automatically fixing composition of other phase in equilibrium with it. Lines joining
points representing compositions of the two phases in equilibrium are called tie lines
which have to be determined experimentally . However, this is out of scope of the
present experiment.
Graphical representation on equilateral triangular coordinates

Suppose the components are denoted using letters A, B, and C. The same
letter will be used to indicate the quantity of a solution or mixture on a phase
diagram. The concentration of ternary liquid system can be plotted on equilateral
triangle coordinates. It is the property of equilateral triangle that sum of perpendicular
distances from any point within the triangle to three sides equals the altitude of the
triangle. We may therefore let the altitude represent 100% composition and distance
to the three sides the percents or fractions of the three components. With reference to
figure, each apex of the triangle represents one of the pure components as marked .
The perpendicular distance from any point such as k to the base AB represents the
percentage of C in the mixture at k, the distance to the base CB, the percentage of A.

52
OBSERVATIONS:
Mixture Benzene Acetic Water Mixture Benzene Acetic Water
No. (ml) acid (ml) No. (ml) acid (ml)
(ml) (ml)
Weight of specific gravity bottle =
Weight of specific gravity bottle + water =
Weight of specific gravity bottle + acetic acid =
Weight of specific gravity bottle + benzene =
Specific gravity of acetic acid =
Specific gravity of benzene =

53
The following are the same as the properties of this graphical representation.
If R g of a mixture at point R is added to the E g of a mixture at E, the new mixture
can be represented or point in which lies on the straight line RE ,such that,
R line ME xE xM
= =
E line RM xM xR
Where xE , xM and xR compositions of any one component in mixture E, M

and R respectively.
Similarly if a mixture at M has been removed from it a mixture of

composition E, the new mixture is on the straight line EM extended in the direction
away from E, and the location of this at R is given by Equation 1.
Different types of ternary liquid systems:

1. Two pairs completely soluble one pair partially soluble;
Example 1: Water (A)-Chloroform (B)-Acetone (C)
Example 2: Benzene (A)-Water (B)-Acetic acid (C)
Liquid C dissolves completely in A and B, but A and B dissolves only to a limited

extent in each other. At a particular temperature and pressure, as shown in figure, a
figure can be drawn for the system. L and K represent saturated liquid mixture of A
and B. Curve LRPEK is the binodal solubility curve. Any mixture outside the curve
will be a homogeneous solution of one liquid phase. A ternary mixture underneath the
curve, such as M, will form two insoluble saturated liquid phases of equilibrium
compositions indicated by R (A-rich) and E (B-rich).The line joining these
equilibrium compositions is called a tie line. And the plot at which the tie line ends is
called plait point. One pair completely soluble - 2 pairs partially soluble.

54
CALCULATIONS:
The volumes of the three components taken in each experiment are converted to
weight fractions
Mixture Weight fraction Mixture Weight fraction
No. Water Acetic Benzene No. Water Acetic Benzene
acid acid

55
Example: Chlorobenzene (A)-Water (B)-Methyl Ethyl Ketone (C)
A and C are completely soluble while pairs A-B and B-C compositions may
show limited solubility. With references to figure 4.3, mixtures such as mixture M are
inside the heterogeneous area and exist as two phases , the compositions of which are
given by points R and E. Line RE is a tie line. Curves KRH and IHEL are ternary
solubility curves and the mixtures outside the band between these curves form
homogeneous single phase liquid solutions.
PROCEDURE
Report the temperature at which the binodal solubility curve is drawn. Wash
the test tubes with water, alcohol or acetone and perfectly dry it by blowing hot air.
Clean the burettes .Distilled water is taken in the burette 1, benzene in burette 2 and
glacial acetic acid in burette 3. Prepare 9 mixtures of varying compositions in h test
tubes by mixing 1cc of water with 9cc of acetic acid, 2 cc of water with 8 cc of acid
and so on. To each mixture add benzene from the bottle drop by drop till turbidity
appears which indicates light traces of separation of new phase. Note down the
volume of benzene added to the mixture.
Wash the test tubes with water and some volatile liquid like alcohol or acetone and
dry it by blowing hot air. Prepare 9 mixtures of varying compositions by taking 1 ml
benzene and 9 ml acetic acid,2ml benzene and acetic acid taken in each is now taken
down. Add water drop by drop till turbidity appears.
To determine points L and K with reference to figure take 10cc of benzene in a clean
dry test tube and find out the volume of benzene needed to make this turbid. Find
specific gravity of benzene and acetic acid using specific gravity bottle.

56

57
RESULT
INFERENCE

58
7. SIMPLE DISTILLATION
OBJECTIVE
To verify Rayleighs equation for simple distillation of methanol water mixture.
To verify material balance equation,
FX F = DYD , Avg + WX W
APPARATUS
1. Simple distillation apparatus.
2. Density bottle
3. Measuring cylinder(10cc)
4. Burette(2No.s)
5. Conical flask (100cc)
CHEMICALS
1. 50 mole% methanol water mixture.
2. Pure methanol
THEORY
Distillation is a method of separating the components of a solution. This
makes use of fact that when part of a liquid mixture is vaporized by addition of heat,
the composition of the new phase may be different from the composition of the
original solution.
Let us consider the addition of heat at constant pressure to a completely
miscible liquid mixture A and B. The temperature of the mixture rises. If it had been
pure A, the vapor pressure of A rises with increases in temperature and finally equals
the pressure at which the operation is carried out. If further heat is added, this is
utilized in converting A from liquid to vapor state at constant temperature. Similar is
the case for component for liquid B also. In other words, we can say that a pure

59
Fig.7.1 Simple distillation experimental setup

60
Component has only one degree of freedom at the two phase equilibrium condition.
But when there are two components, phase rule suggests two degree of freedom for
the same situation, which means that there is a range temperatures through which the
transition from liquid to vapor state occurs. The temperature at which vaporization
starts is called bubble point and the temperature at which the vaporization ends is
called dew point.
In the figure the mole fraction of more volatile component (here A) is used to
denote the compositions of the mixtures. Consider the mixture to be initially in the
liquid phase denoted by point G. On addition of heat, the temperature of the mixture
rises. Let us consider that two components, the state of the system has reached point
H, when the vapor pressure of the solution equals the constant pressure exerted. The
liquid mixture is at the point of vaporization; or the liquid mixture has reached its
bubble point. When more heat is added, the temperature further rises to point P. Now
the system exists in two phases; a liquid phase represented by point L and a vapor
phase represented by point K. The composition of the liquid phase suitably changed
so that the vapor pressure of the solution is equal to the pressure maintained. This is
the property made use of in distillation to effect separation between A and B. On
further addition of heat the state of the system reaches point M where the mixture gets
completely vaporized. The system at this state said to beat at its dew point. The
bottom line is saturated liquid line and the top curve is the saturated vapor curve.
Vapor phase K and liquid phase L coexist and hence they said to be in equilibrium.
While the mole fraction of A in the liquid phase is denoted by x, the mole fraction of
A in the vapor phase in equilibrium which is denoted by y*. If there is a separation by
distillation, y* has to be different from x.

61
OBSERVATIONS
Weight of
Volume of Volume
Mix mix with Density Specific Mol % of
methanol of water
No Sp.gravity (g/ml) gravity Methanol
(mL) (mL)
bottle (g)
10
11
Volume of Methanol-Water mixture for distillation = 400 mL

Volume of distillate collected =
Volume of residue after distillation =

62
Differential or Simple distillation

With reference to the figure, let us consider that the state of the system has
reached the point H. A drop of vapor forms which has compositions represented by J.
By some method this vapor is removed from the vessel in which the equilibrium
distillation is carried out and is condense elsewhere. The composition of liquid phase
moves up along the saturated liquid line. Addition of more heat forms more vapor,
but all vapor is removed from the region of distillation immediately on formation.
The process of distillation is stopped when the composition of the liquid phase has
changed to the extent required. In practice this can only be approximated since,
Removal of differential amounts if vapour makes the process infinitely slow.

Entrainment cannot be fully avoided.
There will be cooling and condensing of the vapour before removal from the
region of distillation.
The amount of liquid that is distilled can be related to the initial and final
liquid phase. Compostion using an equation called Rayleighs equation. For a binary
mixture of a &b assume that at any time during the course of distillation there are l
moles of liquid in the still of composition. X mole fraction of A and the amount of
distillate (=dL) of mole fraction y* in equilibrium with the liquid is formed. Let us
denote the corresponding change in the liquid phase composition by dx.
Let us determine the corresponding material balance for A

Lx = y * dL + ( L dL)( x dx)
Lx = y * dL + Lx Ldx xdL + dxdL
dxdL can be neglected.
y * dL = Ldx + xdL
dL F xF dx
L
= ln =
W xW ( y * x)

63
Sp. Gravity Bottle + Feed Bottle + Bottle +

bottle Distillate Residue
Weight (g)
.
CALCULATIONS
Molecular wt. of methanol = 32

Molecular wt. of water = 18
Specific gravity of feed mixture =
Specific gravity of distillate =
Specific gravity of residue =
Density of methanol = ______________ g/cc
Density of water = 1 g/cc
The equilibrium relation between Methanol (A) Water (B) system at 1 atm :
xA 0 0.02 0.04 0.06 0.09 0.14 0.22 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
y* A 0 0.1 0.2 0.3 0.4 0.5 0.6 0.66 0.73 0.78 0.82 0.87 0.92 0.96 1.0
1 /( y * x)

64
Where F and W are the total number of moles of liquid at any instant during
distillation having composition xf and xw respectively. This equation can be used to
determine F , W , xF and xW for simple distillation when any three of these are
known.
PROCEDURE
1. About 400ml of given methanol-water mixture in a simple distillation flask after
exactly determining the volume using a measuring cylinder. Assemble the distillation
apparatus, start circulation of water through condenser and switch on the heating.
2. Take distilled water in one burette and methanol in another. Determine the specific
gravity of pure methanol. Clean and dry a 100cc conical flask. Prepare a 10% by
volume mixture of methanol and water in this by mixing 3ml methanol with 27ml
water and find out the specific gravity of this mixture.
3. Similarly find the specific gravities of several known compositions of methanol-water
mixtures. It is better to do the experiment in increasing percentages of methanol and
to shake the dry bottle between successive density determinations so that little amount
of solution remaining in the bottle will not affect the experiment much.
4. When about 200cc of distillate has been collected, stop heating and dissemble the
apparatus. Measure the volume of distillate collected in that of residue remaining
using a measuring cylinder. Determine the specific gravities of this solution also.
RESULT
The material balance equation and the Rayleighs equation have been verified for the
given methanol-water system
INFERENCE

65
From graph:
Mole fraction of methanol in the distillate, y D , avg =
Mole fraction of methanol in feed, xF =
Mole fraction of methanol in residue, xW =
For feed, F
Volume of Methanol = 200 mL
Mass of Methanol = Volume Density =
x F Molecular wt. of methanol
Mass fraction of methanol in feed =
x F Molecular wt. of methanol + (1 x F ) Molecular wt. of water
=
=
Mass of feed F = volume of feed specific gravity of feed
=
=
Mass of feed Mass fraction of methanol in feed
Moles of methanol in feed =
Molecular wt. of methanol
=
=
Mass fraction of Water in feed = 1-Mass fraction of methanol in feed
=
Mass of feed Mass fraction of water in feed
Moles of water in feed =
Molecular wt. of water
=
=
Total moles in feed = moles of methanol in feed + moles of water in feed
=

66

67
For distillate, D
From graph: xD = y D , avg =
y D , avg 32
Mass fraction of methanol in D =
y D , avg 32 + (1 y D , avg ) 18
=
=
Mass of distillate D = volume of distillate specific gravity of distillate

=
Mass of distillate Mass fraction of methanol in distillate
Moles of methanol in D =
=
=
Mass fraction of water in D = 1-Mass fraction of Methanol in D
=
Mass of distillate Mass fraction of water in D
Moles of water in D =
18
=
=
Total moles in distillate D = Moles of methanol in D + Moles of water in D
=
For residue, W
From graph: xW =
xW 32
Mass fraction of methanol in W =
xW 32 + (1 xW ) 18
=
=
Mass of residue W = volume of residue specific gravity of residue
=

68

69
Mass of residue Mass fraction of methanol in residue

Moles of methanol in W =
=
=
Mass fraction of water in W = 1-Mass fraction of Methanol in W
=
Mass of residue Mass fraction of water in W
Moles of water in W =
18
=
=
Total moles in residue W = Moles of methanol in W + Moles of water in W
=
From material balance, FxF = Dy D , avg + Wxw
Total moles in feed, F =

Total moles in distillate. D =
Total moles in residue, W =
xF =
xD = y D , avg =
xW =
Substitute the values in the material balance equation and verify.
xF dx
The area under the curve between xF and xW gives the value of
xW ( y * x)
Area under the curve from graph =
F
ln =
W

70
8. SIMPLE STEAM DISTILLATION
OBJECTIVE
To study the characteristics of Steam Distillation using Turpentine oil as a feed
stock.
AIM
To determine vaporization efficiency ( V ) and thermal efficiency ( T )
INTRODUCTION
Steam Distillation is a term used to describe a distillation process with open
steam. It is specifically used where it is desired to separate substances at a
temperature lower than their normal boiling point.
In a steam distillation process, the liquid is distilled by feeding, open steam
to the distillation still. The steam carries with it vapors of volatile liquid and
is then condensed to separate the liquid from water. The essential requirement
for carrying out steam distillation is:
1. Substance does not react with steam.
2. Substance is in-soluble in water.
THEORY
If P is the total system pressure, PA is the vapor pressure of turpentine (A) and
PB is the vapor pressure of water (B), then

P = PA + PB (1)
For atmospheric distillation: P = 101.3 KN/m2

Plot of PA vs T and ( 101.3 PB ) vs T on the same graph gives
Hausbrand Vapour Pressure diagram. The intersection of the two curves
gives the distillation temperature. Let N A be the number of moles of Turpentine
71
Nomenclature
MA = Molecular weight of turpentine
PA = Vapor pressure of turpentine oil, kN/m2
PB = Vapor pressure of steam, kN/m2
Pg = Gauge pressure, kg/cm2

P = Total pressure, kN/m2
WS = Wt. of Steam condensed in the jacket , kg
T1 = Distillation temperature, C
W AD = Wt. of turpentine in distillate, kg
WBD = Wt. of water in distillate, kg
WBB = Wt. of water in residue, Kg
W AF = Wt. of turpentine in feed, Kg
W AB = Wt. of turpentine in Residue, kg
N AF = No. of moles of turpentine oil in feed, g mole
N AD = No. of moles of turpentine oil in distillate, g mole
N AB = No. of moles of turpentine oil in residue, g mole
N BD = No. of moles of water in distillate, g mole
N BB = No. of moles of water in residue, g mole
V = Vaporization efficiency, %
T = Thermal efficiency, %
72
oil in vapor phase. Let N B be the number of moles of Water in the vapor phase.
Partial pressure of turpentine oil in the vapor phase
PAo = P[N A /( N A + N B )] (2)

and Partial
o
pressure of water in the vapor phase,
PBo = P[N B /( N A + N B )] (3)
PAo N A W A / M A
= = (4)
PBo N B WB / M B
Where W A & WB represent the gms or kg of turpentine & water respectively in
the Vapour phase. M A & M B are the corresponding molecular weights. Equation
(4) can be written in terms of vapor pressure as:
WB PBo M B
=
W A PAo M A
(assuming 100% vaporization efficiency)
WB (101.3 PAo ) M B
= (5)
WA PAo M A
Knowing the vapor pressure ( PA ) of turpentine oil (from Hausbrand
Vapour Pressure diagram) at the distillation temp. ( TD ), amount of open steam

required (i.e; amount of steam condensed per unit weight of turpentine condensed in
the distillate) can be computed. The actual steam requirement is higher due to:
1. Steam is used externally to provide the sensible heat for heating the feed
charge from ambient temp. to the distillation temp.
2. Due to heat losses from the still.
3. Due to in-adequate steam-liquid contact, actual state of equilibrium is
difficult to achieve.
Since vaporization efficiency is usually < 1, defining vaporization efficiency V as:
PAo
V =
PA
73
Fig.8.1 Hausbrand vapor pressure diagram of various organic

solvents
OBSERVATION
DATA:
M A = --------------- M B = ---------------
PA = --------------- kN/m2
Pg = ______________ kg/cm2
74
Equation (5) is written as:

WB (101.3 V PA ) M B
= (6)
WA V PA M A
Overall energy balance around the distillation unit shall give the thermal efficiency
Qout
T =
Qin
Qout =W AF(TD TR )C PA + AW AD = WS + AW AD (Neglecting heat losses from the

still)
Qin = WS j + (WBB + WBD )[ S + C P (TS TD )]
DESCRIPTION
In steam distillation setup the feed mixture is filled into the vessel and
steam is supplied for the initial heating of the feed mixture. steam trap is also
provided for optimum use of the steam. A Spurger is provided that is dipped into
the feed. The steam is imp inched into the feed and the vapors of the feed
component is gone out from the vessel and condensed into the heat exchanger.
The continuous cold water supply is given through the Rota meter. Pt-100 sensor
with DTI is provided for not down the temperature at required locations. DTC is
provided for controlling the steam temperature
UTILITIES REQUIRED
1. Electrical supply: Single Phase, 220 V AC, 50 Hz, 3 kw with earth
connection.
2. Water Supply : 4 LPM (approx.)
3. Drain required.
PROCEDURE
1. From the Hausbrand vapor pressure diagram for turpentine water system at
75
Sl. No. W AF ,kg W AD , kg W AB , kg WBB , kg WBD , kg WS , kg T1 ,C
CALCULATIONS
P = Pg 9.8066 10 7 =
= kN/m2
W AF
N AF = , gmol =
MA
W AD
N AD = , gmol =
MA
W AB
N AB = , gmol =
MA
WBD
N BD = , gmol =
MB
WBB
N BB = , gmol =
MB
Material Balance
N AF = N AD + N AB =
76
101.3 kN/m2 pressure, obtain the distillation temperature, T1 , C (95C)

2. Charge the distillation still with 1 kg of turpentine oil.
3. Adjust the jacket steam pressure to 170 kN/m2 ( Pj ) and start the
cooling water supply to the condenser. Record the still temp. Collect the
steam condensed in the jacket.
4. When the temperature in the still reaches 2C below the distillation
temperature ( T1 ), the jacket steam is stopped and the flow of live steam is
started through the steam sparger. The live steam pressure is adjusted
around 150 kN/m2 ( PS ).
5. Weigh the steam condensed in the jacket ( WS ), kg.
6. Continue the distillation process for sufficient time so that about 50-70%
turpentine charged is distilled (around 1 hr).
7. Stop the steam supply and collect the distillate in the 2 L separating funnel.
Allow the formation of organic layer and an aqueous layer. Separate the
two phases and weigh them ( W AD , WBD ), kg.
8. Collect the residue; separate the two layers and weigh W AB , WBB (kg).
9. Stop the supply to the condenser.
RESULT
INFERENCE
77
PAo = P[ N AD /( N AD + N AB )] =
=
PAo
V = =
PA
W AD
% Recovery = 100 =
W AF
VAPOR PRESSURE DATA FOR TURPENTINE OIL

Vapor
Vapor
Temperature pressure of
pressure of 1- PB 101.3- PB PA (kPa )
(C) Turpentine,
Water, PB
PA
60 0.0346 0.1964 0.8036 100.97 3.51
66.5 0.0442 0.2528 0.7472 75.04 4. 478
71 0.0550 0.3223 0.677 68.04 5.572
76.5 0.0686 0.4074 0.5926 60.0 6.95
82 0.0870 0.5106 0.4844 49.56 8.8
87.7 0.1081 0.6350 0.305 36.95 10.95
93.5 0.1339 0.7837 0.2163 21.89 13.56
99 0.1645 0.7603 0.0395 3.99 16.65
104.5 0.2012 1.1686 - - 20.38
110 0.2475 1.4130 - - 25.0778
78
Hausbrand Vapor pressure diagram for Turpentine oil and

Steam
120
101.3-PB
100
PA (kPa)
Vapor Pressure (kPa)
80
60
40
20
0
60 66.5 71 76.5 82 87.7 93.5 99 104.5 110
Temperature (C)
Fig.8.2 Hausbrand Vapor pressure diagram for Turpentine oil and Steam
79

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National Institute of Technology Calicut Department of Chemical Engineering

1. VAPOUR IN AIR DIFFUSION

Study of the effect of temperature on the diffusion coefficient

Diffusion is concerned with the movement of individual molecules through a

CH 3094 Mass Transfer Laboratory Page 1

C B = Molar concentrations of B, k mole/m3

Fig.1.1 Experimental setup

CH 3094 Mass Transfer Laboratory Page 2

Where P A1 and P A2 are the partial pressures of A at the boundaries of the

This is the expression used for the experimental determination of vapour

The rate of evaporation is thus given by:

CH 3094 Mass Transfer Laboratory Page 3

OBSERVATIONS and CALCULATIONS

CH 3094 Mass Transfer Laboratory Page 4

Other form this equation that is convenient to use is:

CH 3094 Mass Transfer Laboratory Page 5

Plot of ( x 0 x) Vs /( x 0 x) from the graph find the slope S

Calculation of vapour pressure, V.P (N/m2) for Acetone at a temperature, T (K)

CH 3094 Mass Transfer Laboratory Page 6

So Relation between temperature & Vapour pressure from this curve

Effect of temperature and pressure on co-efficient of diffusion, D is expressed as:

CH 3094 Mass Transfer Laboratory Page 7

From Graph, S = sec/cm2 = 10-4 sec/m2

CH 3094 Mass Transfer Laboratory Page 8

CH 3094 Mass Transfer Laboratory Page 9

2. WATER COOLING TOWER

CH 3094 Mass Transfer Laboratory Page 1

Air out (G2, T3, T4, H1) Water in (L1, T5)

Air in (G1, T1, T2, H2) Water out (L2, T6)

Fig.2.2 Counter flow Cooling Diagram

CH 3094 Mass Transfer Laboratory Page 2

Then the enthalpy balance is.

The rate of heat transfer from liquid to interface is

The rate of heat transfer from interface to gas is

Where hG & hL = heat transfer coefficient

A = heat transfer area

The enthalpy of the liquid

Where C L = specific heat of liquid

TO = base temperature for computing enthalpy

So, equation for liquid phase heat transfer,

CH 3094 Mass Transfer Laboratory Page 3

OBSERVATION AND CALCULATION:

CH 3094 Mass Transfer Laboratory Page 4

Then, for gas phase heat transfer,

Tower characteristic can be evaluated numerically by :

ha1 = h1 + 0.1( L / G )(T5 T6 )

And hi = hwi hai

CH 3094 Mass Transfer Laboratory Page 5

OVERALL HEAT TRANSFER COEFFICIENT

CH 3094 Mass Transfer Laboratory Page 6

From Enthalpy table,

CH 3094 Mass Transfer Laboratory Page 7

Enthalpy of leaving air (h2) is,

T , F hwi hai hi = hwi hai

T = T6 + 0.4(T5 T6 ) hw = ha = h1 + 0.4( L / G )(T5 T6 )

T = T5 0.4(T5 T6 ) hw = ha = h2 0.4( L / G )(T5 T6 )

T = T5 0.1(T5 T6 ) hw = ha = h2 0.1( L / G )(T5 T6 )

CH 3094 Mass Transfer Laboratory Page 8

5. Record the temperatures.

CH 3094 Mass Transfer Laboratory Page 9

Mass transfer coefficient

hw1 = btu/lb of dry air

hw 2 = btu/lb of dry air

hw3 = btu/lb of dry air