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JCT

Mass transfer laboratory

2013-14

SIMPLE DISTILLATION
Aim:

To verify Rayleighs equation for the given binary system.

Apparatus required:
Simple distillation setup, measuring jar, specific gravity bottle and beaker.
Theory:
In simple distillation, a batch of liquid is charged to a kettle or flask fitted with some
sort of heating device. the charge is boiled slowly and the vapors are withdrawn as rapidly
as they form in a condenser where they are liquefied and the distillate collected in the
receiver the vapor leaving the flask at any time is in equilibrium with the liquid in the flask,
but since the vapor is richer in the more volatile component , the composition of liquid and
vapor are not constant .the first portion of the distillate will be the richest in the more
volatile component and as distillation proceeds ,the vaporized product become leaner, the
distillate can therefore be collected in several separate batches to give a series of distilled
product of various purity.
Rayleighs equation is:

ln F / W

xF

xW

dX
Y X
*

Procedure:
1) Take 200 ml of component A (Acetone) and 100ml of component B (Water) in the
distillation flask and heat over a heating matter.
2) Carry out the distillation until 2/3rd of the mixture get distilled.
3) Collect the distillate in conical flask.
4) Find out the volume of distillate.
5) Cool the residue to room temperature.
6) Find out the volume of the residue.
7) Find out the density of residue using specific gravity bottles.
Observation:
Volume of Acetone taken

ml

Volume of Water taken

ml

Density of Acetone

g/cc

Density of Water

g/cc

Weight of empty specific gravity bottle =

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Mass transfer laboratory

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Tabulation: 1
Calibration Chart:
S.
No.

Volume in ml
Aceton
e

Water

Weight in g
Sp. gr. Bottle
+ Sample

Mole fraction of

Sampl
e

Acetone

Refractive
Index/Specific
gravity of Acetone

Water

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
Calculation:
Weight of Acetone

(Volume of Acetone) * (Density of Acetone)

Weight of Water

(Volume of Water) * (Density of Water)

Moles of Acetone taken (W) =

(Weight of Acetone) / (Molecular Weight of Acetone)

Moles of Water taken (D)

(Weight of Water) / (Molecular Weight of Water)

Total Moles

Moles of Acetone + Moles of Water

Mole Fraction of Acetone (XF) =

Moles of Acetone / Total Moles

Mole Fraction of Water

Moles of Water / Total Moles

Volume of Residue Collected =

ml

Volume of Distillate Collected =

ml

Density of Residue

g/cc

Specific Gravity of Residue

Density of Residue / Density of Water

From the graph Specific Gravity (Y-axis) vs. Mole Fraction of Acetone (X-axis),
Mole fraction of Acetone in Residue, Xw =

Average Molecular Weight of Residue = [Xw * Molecular weight of Acetone] +


[(1- Xw) * Molecular weight of water]
Feed in gmols (F)
=D+W

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Mass transfer laboratory

Residual liquid in gmols (W)

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Tabulation: 2
VLE data for Acetone-Water system:
(Refer Chemical Engineering Handbook by Robert. H Perry & Don Green, 6th edition, Page
Nos: 13.11-13.12 & 13.21)
S.
No.

Y*

Y* - X

1/(Y* - X)

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.

Verification:

Rayleighs equation is

ln F / W

xF

xW

dX
X

From graph X (y-axis) vs. 1/(Y* - X) (x-axis), find the area under the curve between
XF and XW. That is,
xF

xW

dx
Y* X

RHS =

From the calculated data, find

Check LHS=RHS

B.E. Petrochemical Engineering

=
LHS = ln (F/W) =

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Mass transfer laboratory

Analytical Method :
ln (F/W) = ln [(xD xR)/(xD xF)]

Result:
Thus Rayleighs equation is verified.

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JCT

Mass transfer laboratory

2013-14

DIFFUSIVITY MEASUREMENT
AIM
To determine the diffusion coefficient of organic vapor in air at various temperatures.
APPARATUS
Diffusivity cell, stop watch.
THEORY
Some liquid 'A' is taken in a diffusivity cell. The concentration of liquid vapour just
above liquid surface is the vapour pressure of the liquid. If a stream of air is being drawn
along the top edge of the cell, the concentration of liquid vapours there is determined by the
amount of liquid vapour present in atmospheric air. The diffusion that occurs in this case is
diffusion of acetone (A) through stagnant air (B). Since the height of the liquid in the cell is
not maintained constant, a Pseudo Steady State diffusion model may be used.
According to this model ,

D AB=

R T 0 a PBM (X X )
2

2
0

2 P M A t (P A 1P A 2)

Where
D AB = Diffusivity of A in stagnant B, m2/sec.

= Density of diffusing liquid, Kg/m3

= Universal gas constant, 8314 J/Kg mol oK

T0

= Operating temperature, oK

P BM
P

= Total pressure, N/m2

MA

= Molecular weight of diffusing liquid, Kg/Kg mole

PA1
PA2
t
X & X0

= log mean vapour pressure, N/m2

= Vapour pressure at point 1, N/m2


= Vapour pressure at point 2, N/m2
= Time of diffusion, seconds

= Final and initial heights of the liquid, m

DESCRIPTION:

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Mass transfer laboratory

The equipment consists of a T tube made of glass, placed in water bath.


provided with heater.

2013-14
Water bath is

Temperature of the bath is controlled by the digital temperature

controller. Stirrer is given to maintain the constant temperature bath. Air pump is provided
to supply the air, passed through the tube. Change in the liquid level is observed by the
travelling microscope with sliding vernier scale.

PROCEDURE
o
o
o
o

Fill the water bath with water 3/4th of its capacity.


Set the water bath temperature approx 50C
Switch ON the heater and stirrer
Wait till the bath attains the set temperature. Note the steady temperature of

o
o
o

the bath
Fill the T-tube with acetone solution up to two centimeters of the capillary leg.
Note down the initial height of liquid in the capillary
Make the connection with air pump and allow a gentle current of air to flow

o
o
o

over the capillary.


Record the height of liquid in the capillary after every 30 min.
Repeat the experiment for different water bath temperatures.
Repeat the experiment for different organic liquids like: ethanol, toluene and
hexane and CCl4.

DATA:

Total pressure P = 1.01325 105 N/m2


Real gas constant R = 8.314 (N m2) m3 / mole-K
Molecular weight of the liquid MA =
g/mole
Partial pressure of liquid at the top of the tube PA2 = 0 N/m2
Constant A = 15.84
Constant B = 2790.8
Constant C = 226.46

OBSERVATIONS
T = ______________
X0 = ______________
OBSERVATION TABLE
Sl.No.

t (min)

X (cm)

Calculation:

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Mass transfer laboratory

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To calculate the property of organic liquid at temperature TC from data book.

A =
kg/m3
x= X0/100 (m) (initial height of liquid at t1 = 0)
x = X/100 (m)
t1 = t 60 (sec)
T0 = 273 + T (K)

PA1 =

PA1 = PA1 (mmHg) X 133.3 (N/m2)


PB1 =P - PA1
PB2 = P - PA2
PBM = (PB2 PB1) / (ln (PB2 /PB1 )

( A

D AB=

B
)
C +T

(mm Hg)

R T 0 PBM ( X X )
2

2
0

2 P M A t ( P A 1P A 2 )

Calculation Table:
S.No

t1 (sec)

x (cm)

RESULTS
Diffusivity of the given organic liquid in air is calculated.

FORCED DRAFT TRAY DRYER


AIM
To study the drying characteristics of a solid under forced draft condition and
(1)

To calculate the rate of drying

(2)

To calculate the critical moisture content

B.E. Petrochemical Engineering

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Mass transfer laboratory


(3)

To plot the graph of time vs moisture content

(4)

To plot the graph of time vs rate of drying

(5)

To plot the graph of moisture content vs rate of drying

(6)

To plot the graph of mass velocity of air vs rate of drying

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Utilities required:
Forced draft tray dryer, Drying solids: sand/asbestos/silica.
THEORY
In many cases, drying of materials is the final operation in the manufacturing
process, carried out immediately prior to packaging or dispatch. Drying refers to the final
removal of water, and the operation often follows evaporation, filtration or crystallization.
Drying is carried out for one or more of the following reason:
1. To reduce the cost of transport
2. To make a material more suitable for handling
3. To provide definite properties
4. To remove moisture this may otherwise lead to corrosion.
Drying of solids is considered to occur in two stages, a constant rate period followed
by a falling rate period. In the constant rate period, the rate of drying corresponds to the
removal of water from the surface of the solid. The falling rate period corresponds to the
removal of water from the interior of the solid. The rate in either case in dependent on:
Flow rate of air, The solid characteristics and Tray material.
The drying rate of a solid is a function of temperature, humidity, flow rate and
transport properties of drying gas. The rate of drying can be determined for a sample of a
substance by suspending it over an electronic balance in the duct. The weight of the drying
sample can then be measured as a function of time.
Let Ws is mass of solid A is drying area, x is moisture content at any time t. The rate of
drying is given as:
N = - (Ws x)/ (A t)
Where x is moisture content difference and t is time difference.
PROCEDURE:
o
o
o
o
o

Prepare a mixture of known weight of sand and water. (30-50% of water)


Fill the tray with above prepare mixture and note down the sand weight.
Set the temperature of blower, switch on the heater and start the blower.
Adjust the valve V1 and set the flow rate of air.
When the desired conditions of temperature and air velocity are reached
(approx 10-15 min) put tray in the drying chamber.

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Mass transfer laboratory


o
o
o

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Using stop watch check the balance reading at every 3-5 minutes interval.
Continue the experiment till three consecutive reading are unchanged.
Repeat the experiment for different solid material and different air flow rate.

OBSERVATIONS:
Data:

Area of the tray A =


m2
Diameter of the orifice do = 0.026 m
Diameter of pipe dp = 0.052 m
Coefficient of discharge Cd = 0.6
T =
C
Ww =
kg
Ws =
kg

TABULAR COLUMN:
S.No

t (sec)

w (kg)

R (m)

Calculations:

Xt = Ww W/W
W=
kg (Final value of w)
X* = Ww W* / W
X* = Xt X*
X = Xn Xn+1
t = tn+1 tn (n=1,2,3.)

Calculation Table:
S.No

t (min)

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t (min)

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Plot the graph of t vs x.

N= = - (Ws x )/ (A t) kg/ sec m2

a0 = /4

do

m2

ap = /4

d 2p

m2

H = R (w/a-1) m

Qa = Cd

G = Qa

S.No

ao a p

2
p

ao

2 g H

m3/sec

a kg/sec

N (kg/sec m2)

G (kg/sec)

Plot the graph of G vs N

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t (sec)

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Mass transfer laboratory

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Plot the graph of t vs N


Plot the graph of N vs x and determine Xc

RESULT

SIMPLE LEACHING
AIM
To plot the theoretical and actual recovery Vs solvent feed ratio.
APPARATUS
Measuring jar, conical flask, burette, pipette, beaker and stirrer
THEORY
Leaching is the process of removal of a solute or solutes form a solid by the use of a
liquid solvent. It originally refers to the percolation of liquid through a fixed bed, but it is
also used to mean solid liquid extraction generally.

The presence of a solid phase

distinguishes it from liquid extraction. Two steps involved in solid liquid extraction are :
1. Contact of solid and solvent to effect transfer of solute to the solvent and
2. Separation of the resulting solution from the residual solid.

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FORMULA
Y1 = Volume of extract = volume of NaOH* normality of NaOH
Volume of extract
Theoretical recovery =

amount of solvent * 100

Amount of solvent + amount of feed


Solvent to feed ratio
1.

50/50 = 1

X1 = (Y1 * 53 * 50 )/1000

2. 100/50 =2

X2 = (Y2 * 53 * 50 )/1000

3. 150/50 =3

X3 = (Y3 * 53 * 50 )/1000

4. 200/50 =4

X4 = (Y4 * 53 * 50 )/1000

5. 250/50 =5

X5 = (Y5 * 53 * 50 )/1000
% Actual recovery = (X / 5) * 100.

PROCEDURE
About 45 gm of sand and 5 gms of oxalic acid and 100 ml of distilled water are taken
as feed in each of the five beakers.

About 50 ml of water is added to first beaker and

stirred well, allowed to settle. From the supernatant solution 10 ml is pipetted out and is
made upto 100 ml. 10 ml of this solution is used for titrating against 0.2 N NaOH. Sodium
hydroxide is standardised using 0.1N oxalic acid. Then 100 ml of water is added to the
second beaker and the same procedure is repeated. Likewise 150 ml, 200 ml of distilled
water is added respectively to third, fourth and fifth beakers and the same procedure are
repeated.
From this, actual recovery, theoretical recovery and solvent feed ratio are calculated.
A graph of percentage actual recovery and percentage theoretical recovery Vs solvent feed
ratio was plotted.
STANDARDISATION OF SODIUM HYDROXIDE:
Volume of
sodium
hydroxide, ml

Burette reading in ml
Initial

B.E. Petrochemical Engineering

Final

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Volume of Oxalic
acid, ml

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Mass transfer laboratory

Volume of Oxalic acid

Normality of Oxalic acid

Volume of Sodium Hydroxide

Normality of

Sodium Hydroxide

Bottle

Volume of

number

extract

20

20

20

20

20

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Burette readings in ml
Initial

Final

Volume of

Normality of

NaOH (ml)

extract N

RESULT
The theoretical, actual recovery Vs solvent feed ratio was calculated and a graph was
also drawn.
Y
X
%
Recovery

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COUNTER - CURRENT LEACHING


AIM
To study the principles of leaching and to compare the results obtained by leaching
the given sample.
APPARATUS
Conical flask, pipette, burette, measuring jar, glass rod and beaker.
THEORY
Leaching is a process of removing solute or solutes from a solid by the use of liquid
solvent. It is originally referred to percolation of the liquids through a fixed bed. But it also
to mean solid - liquid extraction generally. The presence of a solid phase distinguishes it
from liquid-liquid extraction.

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Two steps are involved in solid - liquid extraction


1. Contact of solid and solvent to effect transfer of solute to solvent.
2. Separation of the resulting solution from the residual solid.
Leaching may be conducted by any of the following methods
Single stage operation
Multi-stage Co-current operation (parallel or cross- current)
In single stage operation the solid feed and the fresh solvent are contacted, mixed
for
Sufficient time for the solute to be transferred to the liquid phase and the solution and the
solids are separated into overflow and underflow respectively. It is rarely encountered in
industrial practice because of low recovery of solute.
In multi stage counter-current system, fresh solvent is added into the first stage and
solid feed is added in the final stage. Underflow from the first stage is sent to the second
stage and so on. The same procedure is repeated in all the succeeding stages.
PROCEDURE
240 gms of sand and 2.5 gms of oxalic acid are taken in a flask labeled 1 to 6. 100
ml of water is added to each. Then 100 ml of water is added to flask (1) and the contents
are shaken and allowed to settle. 100 ml of supernatant liquid is pipetted out into flask (2).
The contents are shaken and allowed to settle, 100 ml of supernatant liquid is pipetted into
flask (3). After the contents are shaken, after settling 100 ml of supernatant liquid from
here is rejected, flask (1) is rejected. The procedure is repeated as shown in the figure until
6th step.
Now, 25 ml of solution, each from flasks 4,5 and 6 are titrated against standard
NaOH solution. The solution of leached solids stage 3 is filtrated into a clean dry conical
flask. 20 cc of this solution is titrated against standard NaOH.
OBSERVATIONS
Amount of oxalic acid taken =
Strength of oxalic acid

STANDARDISATION OF SODIUM HYDROXIDE


Volume of NaOH
pipetted

Burette reading
Initial
Final

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Volume of oxalic
acid used

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Mass transfer laboratory

Strength of NaOH

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= volume of oxalic acid * strength of oxalic acid

Volume of NaOH
Stage Number

Vol. Of sample used

Vol. Of NaOH consumed

RESULT
The result obtained were compared by leaching a given feed
1. Number of stages used

= ___________

2. Number of stages required theoretically = ___________

STAGE WISE LEACHING


Aim:
To separate a solute constituent from a solid mixture by stage-wise leaching.
Apparatus:
500 ml beaker, Funnel, Filter paper, Pipette, Burette, Glass rod.
Chemicals required:
Sodium carbonate, sand, Dilute HCl, Indicator and water.
Procedure:
Take three cleaned and dried 500 ml beaker, it is numbered from 1 to 3.
Into each beaker accurately weighed quantity of 50 g of sand and 20 g of sodium carbonate
was taken.
All beakers are thoroughly mixed with glass rod

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To the first beaker 300 ml of distilled water was added. The contents are stirred well and
allowed to settle. Similarly 150 ml of water added to second beaker and 100 ml of water to
the third beaker respectively.
After the sand particles have settled the clear supernatant liquid was decant into the
corresponding beaker.
The procedure is repeated again with 150 ml of water in second beaker and 100 ml of water
in third beaker.
Finally again 100 ml of distilled water is added to the third beaker.
20 ml of makeup solution from each beaker was titrated against standard HCl.
The amount of Sodium carbonate was calculated in each stage.
Calculation Procedure:
Volume of leached solution V2 = 20 ml
Normality of HCl N1 = 1 N
Stage I:
Volume of HCl added V1 =

ml

Normality of leached solution N2 = V1 N1 / V2

Amount of Sodium carbonate in 1000 ml of solution = ( Equivalent weight Normality


Volume of extract) 100

% Extraction = (Amount of extract/Amount of feed) 100


Tabular Column:
Stages

Volume of leached

Volume of

Burette reading ml

Volume of HCl

solution in ml

extract in ml

Initial

in ml

Final

Result:
Stagewise leaching experiment was performed and percentage extraction was calculated.

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Mass transfer laboratory

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LIQUID-LIQUID EXTRACTION
Aim:
To carryout liquid-liquid extraction for extracting acetic acid from water using solvent and to
find the distribution coefficient and percentage of extraction.
Apparatus Required:
Conical flask, Separating funnel, Burette, Pipette, Measuring Jar
Formulae Used:
Distribution coefficient: Kd = Cd / Cn
Cd Concentration of extractable in organic phase
Cn - Concentration of extractable in water phase
Procedure:
Prepare 1N acetic acid solution and 0.1N NaOH solution. 40 ml of acetic acid and 20 ml
of solvent is taken in a separate flask and stirred using rotary shaker for 15 minutes. Then
the mixture is allowed to separate as layers and pour it into a separating funnel.

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The

JCT

Mass transfer laboratory

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bottom layer raffinate was measured and 20 ml of it is pipette and titrated against NaOH
solution. From the titration value distribution coefficient and % extraction were calculated.
Calculation procedure:
Before extraction:
1. Amount of acetic acid in 40 ml solution of 1N = (Volume of acetic acid Equivalent
weight of acetic acid Normality of acetic acid / 1000)

After extraction:
2. Normality of acetic acid V1 N1 = V2 N2

3. Amount of acetic acid in 40 ml = (Volume of acetic acid Equivalent weight of acetic acid
Normality of acetic acid / 1000)

4. Amount of acetic acid extracted =


5 % of Extraction = (Amount of acetic acid extracted/ Amount of acetic acid in 40 ml)100

6. Distribution coefficient =

Result:
The distribution coefficient and % extraction of various solvents were calculated.

B.E. Petrochemical Engineering

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Mass transfer laboratory

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ROATARY DRYER
OBJECTIVE
To study the operation of rotary dryer.
AIM
To calculate the rate of drying for different air flow rates and different air inlet temperatures.
To plot the rate of drying curve.
Theory:
In many cases, the drying of materials is the final operation in the manufacturing process,
carried out immediately prior to packaging or dispatch.

Drying refers to final removal of

water, & the operation often follows evaporation, filtration or crystallization.

Drying is

carried out for one of the following reasons.

To reduce the transportation cost


To make a material more suitable for handling, for example soap powders, dye

stuffs, fertilizers.
To provide definite properties, such as maintaining free flowing nature of salt.

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To remove moisture; which may otherwise lead to corrosion, for example, the drying
of coal gas or benzene prior to chlorination.

Almost all drying processes involve the removal of water by vaporization, & thus require the
addition of heat.
The rotary dryer is a type of industrial dryer employed to reduce or minimize the liquid
moisture content of the material by bringing it direct contact with a heated gas. The dryer
is made up of large rotating cylinder which slopes slightly so that the discharge end is lower
than the material feed end is order to cover the material under gravity. Material to be dried
enters the dryer as the dryer rotates, the material is lifted up by a series of internal fins
lining the inner wall of the dryer. Heating option include steam, gas, oil, thermal oil, and
auxillary biomass burner system.
Consider a rotary continuous direct heat counter current dryer fed with a nonporous
material having all moisture as unbound moisture. As this material enters the dryer, it is
first heated to the drying temperature.

It will then pass through the length of dryer at

nearly the wet-bulb temperature and theoretically at the end of the dryer, the material shall
be discharged as dry material nearly at the wet bulb temperature.
Assumptions:

NO heat losses from the dryer.


Heat is applied to the material only from the air, not by conduction from the dryer

shell.
All the moisture present is free moisture.
There is no evaporation of moisture in the preliminary heating period.

Drying proceeds at a constant wet bulb temperature until desired amount of water has been
removed. The entering air is assumed to be 100% saturated, so its temperature needs to
be raised so as to decrease the relative saturation.

This would enable the air to absorb

moisture from the wet solid feed. In turn the exiting air is more saturated than the entering
one.
For continuous dryer at steady state operating conditions,
F(X1 X2) = G (Y1 Y2)
This assume that the dry gas flow G and dry solids flow F do not change between dryer inlet
and outlet. Mass balances can also be performed on the overall gas and solids entrainment
in the exhaust gas stream.
The required solids flow rate, inlet moisture content X1 and outlet moisture X0 are normally
specified, and the evaporation rate and outlet gas flow are calculated.
For batch dryer with dry mass m of solids, a mass balance only gives a snapshot at one
point during the drying cycle and an instantaneous drying rate given by:

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m dX/dt = G (Y1 Y2)


dX/dt = G(Y1 Y2) / m
Sometimes dX/dt is called rate of drying.
Description:
The set-up consists of a long resolving cylindrical shell slightly inclined toward the outlet.
The shell is fitted with two brackets for support. Air from a blower passes through a heating
chamber serves the purpose of drying agent. An arrangement is provided for rotating the
dryer shell connected with electric motor and a reduction gear box. Flow control vale and
by-pass valve are fitted to regulate the airflow.
Utilities required:
Solid material (seeds 3-5 mm): 2 kg
Experimental procedure:

Take known amount of the solid material and weigh it.


Now mix known amount of water in the solid and weigh the wet solid.
Set the preheating temperature of air.
Switch ON the blower and set the flow rate of air by adjust the valve V1.
Switch ON the heater & wait till the set point temperature is arrived.
Fill the feed hopper with wet solid.
Start the dryer in rotary motion.
Allow the wet solid to flow through the dryer by starting the screw conveyor and

rotating hand wheel manually.


At steady state record the manometer reading.
Note down the air temperature at inlet Sand outlet.
Repeat the experiment for different air flow rates.
Repeat the experiment for different air inlet temperature.

Observation & Calculation:


Data:
Area of the dryer A
Diameter of orifice do
Diameter of pipe dp
Coefficient of discharge Cd
Acceleration due to gravity g
Density of water and air
Molecular weight of air and water

m2
0.026 m
0.052 m
0.64
9.81 m/sec2
1000 & 1.21 kg/m3
29 & 18 g/mole

Observations:
Z0 =

kg

Z=
W=

kg
kg

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T=

2013-14

sec

S.No

T1 (C)

T2 (C)

T3(C)

T4 (C)

h1 (cm)

Calculations:

H=

h1 h2 w
1 m
100 a

a1= d 2P ( m2)
4

a2= d 2o ( m2 )
4
Q a=

G=

a1 a2

a a
2
1

2
2

C d 2 g H

a Q a
( kg/m2 sec )
A

X = Z Z0/W kg moisture / kg dry solid


To calculate the humidity (y1 & y2) of air at temperature (T1 & T2) and (T3 & T4) respectively
by psychometric chart.
y1 =
y2 =
Y1 = y1 (Mw / MA) (kg of moisture/ kg dry air)
Y2 = y2 (Mw / MA) (kg of moisture / kg dry air)
Y = Y1 Y2 (kg of moisture / kg dry air)
NC = G Y 1000 / (W X) (kg of moisture / m2 sec)

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S.No

Mass transfer laboratory

t (sec)

B.E. Petrochemical Engineering

N ( kg of moisture / m2 sec)

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