National Institute of Technology Calicut

----------------------------A Deemed University---------------------------------

NITC CAMPUS P.O., KERALA – 670 601, INDIA

Department of Chemical Engineering

Laboratory Record

Name: ROHIT.S.ANTARAGANGI

Class: Year: 2021-2022

Roll No:

Reg. No.: B181123CH

Certified that this is the bonafide record of the work done in CH 3094 Mass Transfer
Laboratory, of this department, at National Institute of Technology, Calicut, by

Mr./Miss:

Place:

Date: Faculty – in – Charge

 INDEX

SL Name of Experiment Date Pg.

Marks Remarks
No No
1 Ternary Liquid Equilibrium 10-08-21 01-08

2 Simple Distillation 17-08-21 09-25

3 Adsorption Isotherm 22-08-21 26-34

4 Simple Leaching 05-09-21 35-44

5 Forced Draft Tray Dryer 22-09-21 45-54

6 Counter Current Leaching 29-10-21 55-63

7 Vapor in Air Diffusion 13-10-21 64-73

8 Simple Steam Distillation 19-10-21 74-82

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Experiment No: Date:

TERNARY LIQUID EQUILIBRIUM

OBJECTIVE

To draw the binodal solubility curve for the system Benzene (A) – Water (B) – Glacial
acetic acid(C) 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

 There are at least three substances and two-phase involved.

 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)
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Figure 1: Ternary liquid equilibrium data represented on equilateral triangular

coordinates.

(a) (b)

Figure 2: (a) Type 1 System (b) Type 2 System

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 Compositions in which the system exists in two phases.

Hence in liquid extraction design, it is important to determine the compositions at which

the system changes from a completely miscible into a two-phase system. If all
compositions of the 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 a binodal curve.

At a given condition of temperature and pressure, the composition of one phase

automatically fixes the composition of another 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 the scope for
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 1, 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.

The following are some of 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 by the point M which lies on the straight line RE, such that,

𝑅 𝑙𝑖𝑛𝑒 𝑀𝐸 𝑥𝐸 − 𝑥 𝑀
= = (1)
𝐸 𝑙𝑖𝑛𝑒 𝑅𝑀 𝑥𝑀 − 𝑥𝑅

where, xE, xM, and xR represents the 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.
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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 dissolve only to a limited

extent in each other. At a particular temperature and pressure, as shown in the
figure, a figure can be drawn for the system. L and K represent a 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.

2. One pair completely soluble - 2 pairs partially soluble.

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

1. Report the temperature at which the binodal solubility curve is drawn.

2. Wash the test tubes with water, alcohol or acetone and perfectly dry it by
blowing hot air.
3. Clean the burettes. Distilled water is taken in the burette 1, benzene in burette 2
and glacial acetic acid in burette 3.
4. 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.
5. To each mixture add benzene from the bottle drop by drop till turbidity appears
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which indicates light traces of separation of a new phase.

6. Note down the volume of benzene added to the mixture.
7. Wash the test tubes with water and some volatile liquid like alcohol or acetone
and dry it by blowing hot air.
8. 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.
9. Add water drop by drop till turbidity appears.
10. 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 water needed to make this turbid
and take 10cc of water in a clean dry test tube and find out the volume of
benzene needed to make this turbid.
11. Find specific gravity of benzene, water and acetic acid using specific gravity
bottle.
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Experiment No: Date:

SIMPLE DISTILLATION

OBJECTIVE

To verify Rayleigh’s equation for simple distillation of methanol-water mixture.

To verify material balance equation, 𝐹𝑥𝐹 = 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

the 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 vapour 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 vapour state at a constant temperature. Similar is the case
for a 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 degrees of freedom for the same situation,
which means that there is a range temperature through which the transition from liquid
to vapour state occurs. The temperature at which vaporization starts is called ‘bubble
point’ and the temperature at which the vaporization ends is called ‘dew point’.
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Figure 1: Simple Distillation experimental setup

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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 have reached point H when the
vapour 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 vapour phase represented by
point K. The composition of the liquid phase suitably changed so that the vapour
pressure of the solution is equal to the pressure maintained. This is the property made
use of in distillation to effect a 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 vapour curve. Vapour 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 vapour phase in equilibrium
which is denoted by y*. If there is a separation by distillation, y* has to be different
from x.

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 vapour forms which has compositions represented by J. By some
method this vapour 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 vapour, but all vapour is
removed from the region of distillation immediately on the 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
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composition using an equation called Rayleigh’s equation. For a binary mixture of A

and 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

Neglect dxdL,

𝑦∗𝑑𝐿 = 𝐿𝑑𝑥 + 𝑥𝑑𝐿

𝑑𝐿 𝐹 𝑥𝐹 𝑑𝑥
= ln =∫
𝐿 𝑊 (𝑦∗ − 𝑥)
𝑥𝑊

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. Add about ml of the 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.
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4. When a requires amount (usually 50% of feed volume) of distillate has been
collected, stop heating and disassemble 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.
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Experiment No: Date:

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 the equation for
adsorption at room temperature.

APPARATUS

Reagent bottles, conical flasks, filtering funnel, burette, pipette, and 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
vapours 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 the 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 a mixture of aromatics
and paraffinic hydrocarbons.

Adsorption can be physical or chemical. Physical adsorption or Vander Waal’s

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 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
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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 fuller’s 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 between 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”.

Figure Adsorption Equilibria

In liquid adsorption, isotherms are important since no appreciable volume changes of

the liquid occur which might be used as a measure of adsorption.

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 the adsorbent. V cm3 of solution/g of adsorbent. As a result of
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preferential adsorption of solute, the solute concentration of the solution is observed to

fall from initial C0 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(C0 -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 (𝐶0 − 𝐶∗)] (1)

where k and n are constants at a particular temperature. It is to be noted that ‘n’ is

independent of units used and ‘ k ’ has units same as that used for C0 or C*. 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

1. Record the room temperature.

2. Weigh about 25 g of Acetic acid exactly in weighing bottle and transfer it
completely by repeated washings to a 250 ml volumetric flask (F1 ) and make
up the volume with distilled water.
3. Pipette out 10 ml of this solution into another 250 ml volumetric flask (F2) and
the volume is made up.
4. Weigh about 5 g of activated carbon into a reagent bottle (B1) by differential
weighing.
5. Add 200 ml of solution from the flask (F2) to this bottle.
6. Repeat the same procedure with bottle numbers B2, B3, B4, B5 with the
difference that the volumes of solution pipette out from the flask F1 are 20 ml,
30 ml, 40 ml and 50 ml respectively.
7. Shake the bottles well for one hour using bottle shaker for adsorption to come
into equilibrium.
8. Prepare a standard solution of Oxalic acid (0.1 N) and use this to standardize
the supplied NaOH solution.
9. After 1 h shaking, filter the solution and titrate in the five bottles. Take the
solutions in the burette and titrate it against 10 ml NaOH.
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Experiment No: Date:

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

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
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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

 The solids leaving the stage retain some of the solutes.

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.

PROCEDURE

1. Varying solvent to feed ratio

i. 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.
ii. Prepare five different feed sample in 500 cc beaker. Now, add an additional
50 cc of distilled water to the beaker. Stir the mixture well and allow the
sand to settle for a few minutes.
iii. 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.
iv. 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.
v. Note that the solvent to feed ratio by volume used in the above experiment
is on sand (unit) free basis.
vi. 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.
vii. In each case, do a suitable dilution of extract before it is titrated against HCl
taken in the burette.
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2. Varying number of stages

i. 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.
ii. Extract the solute from each beaker with 200cc of water but with varying
number of stages from 1 to 5.
iii. 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
iv. 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 clear solution and mix it with the earlier
extract. Find strength of this combined extract by titrating against 0.1 N HCl
solution.
v. Beaker 3: Extracted 3 times using 66.6cc of water each time.
vi. Beaker 4: Use 50cc of water four times.
vii. Beaker 5: Use 40cc of water five times.
viii. 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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Experiment No: Date:

FORCED DRAFT TRAY DRYER

OBJECTIVE

To study the drying characteristics of a solid under forced draft condition.

AIM

To determine the drying rate of a solid under forced draft condition and determine the
critical moisture content.

INTRODUCTION

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.

THEORY

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, is dependent
on:

 Flow Rate of Air.

 The Solid Characteristics.
 Tray Material.

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.
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NOMENCLATURE

A = Drying surface area, m2

ao = Area of orifice, m2

aP = Area of pipe, m2

D = Diameter, m

do = Diameter of orifice, m

dp = Diameter of pipe, m

G = Mass flow rate of air, kg/s

h = Head loss, m

N = Drying rate, kg/m2 s

W = Weight of moist solid, kg

Nc = Constant drying rate, kg/m2 s

R = Manometric difference, m

S = Weight of dry solid, kg

X = Moisture constant of a solid, kg of water/kg of dry solid

Xc = Critical moisture content.

θ = Time, s

ρa = Density of air, kg/m3

ρw = Density of water, kg/m3

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Let the weight of dry solid =S

Let the weight of dry solid + moisture =W

Then, kg of water/kg of dry solid =X

W−S
X=
S

Drying Rate N (kg/s m2)

S Δx
N=−
A Δθ

A = exposed surface area for drying, m²

DESCRIPTION

The set up consists of an insulated double wall chamber. Inside the chamber, a tray is
attached directly to an electronic weighing balance, which is fitted on bottom outside
the chamber. Material for drying is placed in the tray and regular loss of weight is
monitored. Air from a blower passes through a heating chamber is used as a drying
agent. Flow control and bypass valve are fitted to regulate the airflow.

UTILITIES REQUIRED

1. Electricity Supply: Single Phase, 220V AC, 50Hz, 5-15 amp. socket with earth
connection.
2. Bench Area Required: 0.75 m x 2 m.
3. Wet Solid.

EXPERIMENTAL PROCEDURE

1. Load the pre-weighed tray with solid and place it over the balance in the drying
chamber.
2. Record the weight of sand & tray.
3. Start the blower and fix the air flow rate and also its inlet temperature by
adjusting the energy regulator.
4. When the desired conditions of temperature and air velocity are reached (in
about 10-15 min), remove the sample tray and put known amount of water in it
to give desired initial moisture content.
5. Keep the tray gently in the drying chamber and start the stopwatch.
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Figure 1: Drying Rate Curve

)
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6. Record the balance reading with time at about 3-5 min interval.
7. Drying is assumed to be complete when at least 3 consecutive readings are
unchanged. The wet/dry bulb temperatures at the inlet and outlet of the drying
chamber and the air flow rate (manometer reading fixed across the orifice) are
recorded at least three times during the course of a run to give average operating
conditions.
8. The same steps are repeated for other runs at different operating conditions.
9. Plot drying rate N (kg/m2 s) vs moisture content X (kg of water/kg of dry solid)
(Drying curve). From this plot, critical moisture (Xc) content is obtained.
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Experiment No: Date:

COUNTER CURRENT LEACHING

OBJECTIVE

To find the overall efficiency of a counter current leaching unit by batch simulation of
a counter 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 stagewise 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 n-th 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) th 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. So the definition of ‘overall stage efficiency’,
notation scheme and the graphical representation is same as of the number of stages.
 P a g e | 56

Counter Current Cascade Arrangement

 P a g e | 57

PROCEDURE

1. Weigh about 50 g of Na2CO3 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.
2. 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.
3. 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.
4. 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.
5. 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.
6. Now the leaching process is continued as shown in Fig. 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.
7. 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.
8. A standard solution of 0.1 N Na2CO3 is prepared and this is used to standardize
the HCl solution used.
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 P a g e | 64

Experiment No: Date:

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 nonuniform. 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 a 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 NB are equal but have
opposite sign.

According to Dalton’s law, the total concentration of the two components CA and CB is
constant

𝑑𝐶𝐴 𝑑𝐶𝐵
=−
𝑑𝑥 𝑑𝑥

Then using the integrated form of the Fick’s Diffusion equation

𝐷 𝐷
𝑁𝐴 = (𝑃𝐴1 − 𝑃𝐴2) = 𝑁𝐵 = (𝑃𝐵1 − 𝑃𝐵2)
𝑅𝑇𝑥 𝑅𝑇𝑥

where PA1 and PA2 are the partial pressures of A at the boundaries of the zone of
diffusion and x is the distance over which diffusion occurs., CA = Molar concentration
of A, k mole/m3
 P a g e | 65

NOMENCLATURE

CB = Molar concentrations of B, k mole/m3

CT = Total molar concentration, k mole/m3

CBM = Log mean concentration of CH3 -CO-CH3, k mole/m3

DAB = Diffusion coefficient, m2 /s

MA = Molecular weight of CH3-CO-CH3 (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 the top end of the tube after time θ, cm

x0 = Initial height from the top end of the tube, cm

x0 –x = Drop in liquid (CH3 -CO-CH3 ) level in time θ, cm

θ = Time of evaporation, s

ρl = Density of CH3-CO-CH3, kg/m3

S = slope of graph s/cm

Figure 1 Experimental Setup

 P a g e | 66

In the case where gas A is diffusing through stagnant gas, B (non-diffusing) the flow
carries both components in proportions to their partial pressure

𝑁𝐴𝑃𝐴 𝑁𝐵𝑃 𝐵
= −
𝑃 𝑃

The total transfer of A is the sum of this proportion of the flow and the transfer by
diffusion

𝑃𝐴 𝐷 𝑑𝑃𝐴
𝑁𝐴 = 𝑁𝐴 −
𝑃 𝑅𝑇 𝑑𝑥
𝑃𝐵 𝐷 𝑑𝑃𝐵
𝑁𝐴 = 𝑁𝐴 (1 − )+
𝑅𝑇 𝑅𝑇 𝑑𝑥
𝑥 𝑃𝐵2
𝐷𝑃 𝑑𝑃𝐵
𝑁𝐴 ∫ 𝑑𝑥 = ∫
𝑅𝑇 𝑃𝐵
0 𝑃𝐵1

𝐷𝑃 𝑃𝐵2
𝑁𝐴 = 𝑙𝑛
𝑅𝑇𝑥 𝑃𝐵1

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 the 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 an appreciable change of level, the value of x is
determined by the integration between the initial and final readings of the level.

The rate of evaporation is thus given by:

𝐷𝑃 𝑃𝐵2 𝜌𝑙 𝑑𝑥
𝑁𝐴 = 𝑙𝑛 =
𝑅𝑇𝑥 𝑃𝐵1 𝑀 𝑑𝜃

Integration of this expression yields:

𝜃 𝑥2
𝐷𝑃 𝑃𝐵2 𝑀
𝑙𝑛 ∫ 𝑑𝜃 = ∫ 𝑥 𝑑𝑥
𝑅𝑇 𝑃𝐵1 𝜌𝑙
0 𝑥1

𝐷𝑃 𝑃𝐵2 𝑀𝜃 𝑥22 − 𝑥12

𝑙𝑛 =
𝑅𝑇 𝑃𝐵1 𝜌𝑙 2
 P a g e | 67

Therefore,

𝑅𝑇 𝜌𝑙 𝑥 2 − 𝑥21
𝐷= ( ) 2
𝑃𝐵2 𝑀 2𝜃
𝑃 𝑙𝑛 𝑃
𝐵1

Other form this equation that is convenient to use is:

𝜌𝐴 (𝑥2 − 𝑥2)𝑅𝑇𝑃𝐵𝑀
0
𝐷𝐴𝐵 = (1)
2𝑃(𝑃𝐴1 − 𝑃𝐴2)𝑀𝐴𝜃

In terms of concentration terms the expression for D is:

2𝜃𝑀𝐴𝐷𝐴𝐵𝐶𝐴𝐶𝑇 (2)
(𝑥2 − 𝑥2) =
0 𝜌𝐴 𝐶𝐵𝑀

𝐶𝐵1 − 𝐵𝐵2
𝐶𝐵𝑀 =
𝐶
ln 𝐵1
𝐶𝐵2

Usually, x0 will not be measured accurately nor is the effective distance for
diffusion, x, at time θ. Accurate values of (x – x0 ) are available, however,
and hence:

Rewriting Eq.2 as:

𝜃 𝜌𝐴 𝐶𝐵𝑀 𝜌𝐴 𝐶𝐵𝑀
= (𝑥 − 𝑥0 ) + 𝑥 (3)
𝑥 − 𝑥0 2𝑀𝐴𝐷𝐴𝐵𝐶𝐴𝐶𝑇 𝑀𝐴𝐷𝐴𝐵𝐶𝐴𝐶𝑇 0

A graph between θ / (x – x0) and (x – x0) should yield

𝜌𝐴 𝐶𝐵𝑀
𝑆= (4)
2𝑀𝐴𝐷𝐴𝐵𝐶𝐴𝐶𝑇
𝜌𝐴 𝐶𝐵𝑀
𝐷𝐴𝐵 = 2𝑀 𝑆𝐶 𝐶 (5)
𝐴 𝐴 𝑇

To determine the total concentration

𝑃
𝐶𝑇 =
𝑅𝑇
Then
(𝑉𝑃)𝐴
𝐶 = [ ] × 𝐶 , at operating temperature T.
𝐴 𝑃 𝑇

CB1 shall be equal to CT.

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𝑃− (𝑉𝑃)𝐴 3
𝐶𝐵2 = [ ] × 𝐶𝑇 , kmol/m
𝑃

Effect of temperature and pressure on the coefficient 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. The 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 (35 °C and 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 (CH3-CO-CH3) up to within two centimeters of the
top of the capillary leg. Note down the initial diffusion height of liquid in the
capillary
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, CCl4, hexane etc. and
tabulate the results and discuss.
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Experiment No: Date:

SIMPLE STEAM DISTILLATION

OBJECTIVE

To study the characteristics of Steam Distillation using turpentine oil as a feedstock.

AIM

To determine vaporization efficiency (ηV) and thermal efficiency (ηT).

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 vapours 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 insoluble in water.

THEORY

If P is the total system pressure, PA is the vapour pressure of turpentine (A) and P B is
the vapour pressure of water (B), then

𝑃 = 𝑃𝐴 + 𝑃𝐵

For atmospheric distillation: P = 101.3 KN/m2

Plot of P A 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 NA be the number of moles of turpentine and NB be the number of moles of water
in the vapour phase.

∴ Partial pressure of turpentine oil in the vapour phase

𝑁𝐴
𝑃0 = 𝑃 [ ]
𝐴 𝑁𝐴 + 𝑁𝐵
 P a g e | 75

Nomenclature

MA = Molecular weight of turpentine

PA = Vapour pressure of turpentine oil, kN/m2

PB = Vapour pressure of steam, kN/m2

Pg = Gauge pressure, kg/cm2

P = Total pressure, kN/m2

WS = Wt. of Steam condensed in the jacket, kg

TD = Distillation temperature, °C

WAD = Wt. of turpentine in distillate, kg

WBD = Wt. of water in distillate, kg

WBB = Wt. of water in residue, kg

WAF = Wt. of turpentine in feed, kg

WAB = Wt. of turpentine in Residue, kg

NAF = No. of moles of turpentine oil in feed, g mole

NAD = No. of moles of turpentine oil in distillate, g mole

NAB = No. of moles of turpentine oil in residue, g mole

NDB = No. of moles of water in distillate, g mole

NBB = No. of moles of water in residue, g mole

ηV = Vaporization efficiency, %

ηT = Thermal efficiency, % oil in vapour phase

 P a g e | 76

and partial pressure of water in the vapour phase,

𝑁𝐵
𝑃0 = 𝑃 [ ]
𝐵 𝑁𝐴 + 𝑁𝐵

𝑃𝐴0 𝑁𝐴 𝑊𝐴 𝑊𝐵
= = ⁄
𝑃𝐵0 𝑁𝐵 𝑀𝐴 𝑀𝐵

Where WA and WB represent the g or kg of turpentine and water respectively in the

vapour phase. MA and MB are the corresponding molecular weights. The previous
equation can be written in terms of vapour pressure as:

𝑊𝐵 𝑃𝐵0𝑀𝐵
=
𝑊𝐴 𝑃𝐴0𝑀𝐴

(assuming 100% vaporization efficiency)

𝑊𝐵 (101.3 − 𝑃𝐴0)𝑀𝐵
=
𝑊𝐴 𝑃𝐴0𝑀𝐴

Knowing the vapour pressure (PA) of turpentine oil (from Hausbrand Vapour Pressure
diagram) at the distillation temperature (T D), the 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 temperature to the distillation temperature.
2. Due to heat losses from the still.
3. Due to in-adequate steam-liquid contact, the actual state of equilibrium is
difficult to achieve.

Since vaporization efficiency is usually < 1, defining vaporization efficiency ηV as:

𝑃𝐴0
𝜂𝑉 =
𝑃𝐴

𝑊𝐵 ( 101.3 − 𝜂𝑉𝑃𝐴0)𝑀𝐵
=
𝑊𝐴 𝜂𝑉𝑃𝐴0𝑀𝐴

An overall energy balance around the distillation unit shall give the thermal efficiency

𝑄𝑜𝑢𝑡
𝜂𝑇 =
𝑄𝑖𝑛
 P a g e | 77

Figure 1: Hausbrand Vapour Pressure diagram of various organic solvents

OBSERVATIONS

DATA

MA =

MB =

PA =

Pg =

TD =

Specific heat of turpentine oil, CPA =

Specific heat of water, CP =

Latent heat of fusion of turpentine oil, λA =

Latent heat of fusion of water, (λj , λS) =

Steam temperature, TS =
 P a g e | 78

𝑄𝑜𝑢𝑡 = 𝑊𝐴𝐹(𝑇𝐷 − 𝑇𝑅)𝐶𝑃𝐴 + 𝜆𝐴𝑊𝐴𝐷 = 𝑊𝑆𝜆 + 𝜆𝐴𝑊𝐴𝐷

Neglecting heat losses from the still,

𝑄𝑖𝑛 = 𝑊𝑆𝜆𝑗 + (𝑊𝐵𝐵 + 𝑊𝐵𝐷)[ 𝜆𝑆 + 𝐶𝑃(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. A steam trap is also provided for the 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 vapours of the feed component are gone out from the vessel
and condensed into the heat exchanger. The continuous cold water supply is given
through the Rotameter. 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, 220V AC, 50 Hz, 3 kW with earth connection.
2. Water Supply: 4 LPM (approx.)
3. Drain

PROCEDURE

1. From the Hausbrand vapour pressure diagram for turpentine water system at
101.3 kN/m2 pressure, obtain the distillation temperature, TD °C ( ≅ 95 °C )
2. Charge the distillation still with 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 2 °C below the distillation temperature
(TD), the jacket steam is stopped and the flow of live steam is started through
the steam sparger. The live steam pressure is adjusted to 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 hour).
7. Stop the steam supply and collect the distillate in the 2 L separating funnel.
 P a g e | 79

8. Allow the formation of organic layer and an aqueous layer. Separate the two
phases and weigh them (WAD, WBD), kg.
9. Collect the residue; separate the two layers and weigh WAD, WBD (kg).
10. Stop the supply to the condenser.
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