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OBJECTIVE
AIM
To determine the diffusion coefficient of an organic vapour (Acetone) in air
INTRODUCTION
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
NOMENCLATURE
AIR (B)
(x0 x )
Acetone
(A)
DP p
NA = ln B 2
RTx p B1
R = ______________ kN.m/kmol.K
l = ______________ kg/m3
MA = ______________kg/kmol
T = ______________ K
OBSERVATION
x0 = _____________ cm
Observation Table:
Sl No. , sec x , cm
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
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
CALCULATIONS:
(x 0 x ), /(x 0 x )
Sl No.
cm sec/cm
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 )
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.
P
CT = , kmol / m 3 =
RT
= k mol/m3
VP
C A = CT , kmol / m 3 =
P
= k mol/m3
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
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
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.
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Packing
Cooling
Tower
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(Where H L & H G are the enthalpies of liquid and gas phase respectively)
These above equation can be simplified and rearranged to find out the heat transfer
coefficient.
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OBSERVATION TABLE:
Sl T1 , C T2 , C T3 , C T4 , C T5 , C T6 , C R1 , cm , R2 , cm Qw
No. LPH
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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
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 )
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CALCULATIONS:
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
= _______________
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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
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The enthalpy of entering air at a wet bulb temperature ( T2 , C )
h1 = ha = ________________
h2 = ha = h1 + ( L / G )[T5 T6 ] =
= ________________________
T = T6 = hw = ha = h1 =
T = T6 + 0.1(T5 T6 ) hw = ha = h1 + 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.
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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
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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 =
T6 , C = _______________ C = ________________ F
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 ) =
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RESULTS
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=________________________
KaV T5 dT T T 1 1 1 1
= = 5 6 + + +
L T6 h h
w a 4 h1 h2 h3 h4
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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
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OBSERVATIONS
Room Temperature = _________ C
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
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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
g adsorbed/ g of adsorbent
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CALCULATIONS
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
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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)
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 )
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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*) =
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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
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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
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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
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OBSERVATIONS
Solvent used
Beaker Sodium in extraction Solvent to
No. Carbonate(gm) Sand(gm) Water(ml) (ml) feed ratio
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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.
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PROCEDURE
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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 =
Normality of extract =
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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.
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Vol. of extract
Theoretical % recovery = 100
Vol. of liquid when feed and solvent are mixed
In the graph theoretical & actual % recovery are plotted on the y axis against the
solvent to feed ratio taken in the x axis.
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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
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Normality of extract, N =
R 1 = (E 1 /V 1 )100 =
R 2 = (100-R 1 )(E 2 /V 1 ) =
In the graph the theoretical and actual % recoveries are plotted against number of
stages.
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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.
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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
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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.
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National Institute of Technology Calicut Department of Chemical Engineering
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.
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RESULT
The fractional efficiency of the leaching process is ________.
INFERENCE
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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
= N
= gm
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= N
Normalityof So ln 53 50
Wt. of Na2CO3 in 200mL of So ln adhearing to leached So ln =
1000
= gm
50
50
= 500 = 0.0909
50
50 + 50
500
=
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 )
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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.
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.
OBSERVATIONS:
Mixture Benzene Acetic Water Mixture Benzene Acetic Water
No. (ml) acid (ml) No. (ml) acid (ml)
(ml) (ml)
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
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
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.
RESULT
INFERENCE
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
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.
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
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.
.
CALCULATIONS
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)
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
From graph:
Mole fraction of methanol in the distillate, y D , avg =
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
=
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
=
=
xW 32
Mass fraction of methanol in W =
xW 32 + (1 xW ) 18
=
=
Mass of residue W = volume of residue specific gravity of residue
=
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
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
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National Institute of Technology Calicut Department of Chemical Engineering
Nomenclature
MA = Molecular weight of turpentine
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National Institute of Technology Calicut Department of Chemical Engineering
oil in vapor phase. Let N B be the number of moles of Water in the vapor phase.
PAo N A W A / M A
= = (4)
PBo N B WB / M B
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
PAo
V =
PA
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National Institute of Technology Calicut Department of Chemical Engineering
M A = --------------- M B = ---------------
PA = --------------- kN/m2
Pg = ______________ kg/cm2
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National Institute of Technology Calicut Department of Chemical Engineering
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
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National Institute of Technology Calicut Department of Chemical Engineering
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 =
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National Institute of Technology Calicut Department of Chemical Engineering
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
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
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National Institute of Technology Calicut Department of Chemical Engineering
PAo = P[ N AD /( N AD + N AB )] =
=
PAo
V = =
PA
W AD
% Recovery = 100 =
W AF
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National Institute of Technology Calicut Department of Chemical Engineering
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