1.

Studies on hydrodynamics in a Packed Bed Tower

Aim:
To study the relationship between pressure drop and gas flow rates and liquid flow
rates.
Objectives:
To study about loading and flooding conditions of packed column
Scope to learn through equipment:
1) To know types of packing, packing characteristics.
2) To learn absorption concept.
3) To know design features of packed column
Theory:
Packed towers used for continuous contact of liquid and gas in both counter current
and co current flow, are vertical columns which have been filled with pickings or devices
of large surface. The liquid is distributed over, and trickles down through, the packed bed,
exposing a large surface to contact the gas.
For most random packings, the pressure drop suffered by the gas is influenced by
the gas and the liquid flow rates. At a fixed gas velocity, the gas pressure drop increases
with increased liquid rate, principally because of the reduced free cross section available
for flow of gas resulting from the presence of the liquid. In the region of figure 1 below A,
the liquid hold up, i.e. the quantity of liquid contained in the packed bed is reasonably
constant with changing gas velocity, although it increases with liquid rate. In the region
between A and B, the liquid hold up increases rapidly with gas rate, the free area for gas
flow becomes smaller, and the pressure drop rises more rapidly. This is known as loading.
As the gas rate is increased to B at fixed liquid rate, the following changes occur.
1. A layer of liquid, through which the gas bubbles may appear at the top of the
packing
2. liquid may fill the tower, starting at the bottom or at any intermediate restriction
such as a packing support so that there is a change from gas-continuous liquid
dispersed to liquid continuous gas dispersed (inversion) or
3. Slugs of foam may rise rapidly upward through the packing. At the same time,
entrainment of liquid by the effluent gas increases rapidly and the tower is flooded.
The gas pressure drop then increases very rapidly. The change conditions in region
A to B of figure 1 is gradual and initial loading and flooding are frequently
determined by the change in slope of pressure drop curves rather than through any
visible effect. It is not practical to operate a tower in a flooded condition; most
towers operate just below or in the lower part of the loading region.
1
Utilities required:
1. Compressed air supply
2. Water supply
3. Drain
Experimental setup
1. The experimental set up consists of a glass column 50 mm I.D. and 600 mm in
length which is mounted vertically on a stand using support plates.
2. The material of construction of all lines and pipe fittings is galvanized iron of the
valves and pressure tapings are of brass.
3. At the bottom of column, a water seal is provided to prevent the leakage of air.
4. A rotameter is installed to measure flow rate of water.
5. The air inlet is connected to balance designed to give steady flow rate of air. An
orifice meter is connected to calibrated mercury U Tube Manometer to measure
flow rate of air.
6. Packing material is Raschig ring of Outer dia 12 mm and Inner dia of 6 mm.
2
Experimental Procedure:
1. Fill feed tank with water.
2. Allow air to pass the column.
3. Measure the pressure drop of air in the U-Tube manometer.
4. Make seven or eight runs of different air flow rates with no water flow.
5. Allow water to pass the column.
6. Allow water to flow in the column along with air at different flow rate for each air
flow rate of air as in step 3
7. Allow the column to reach steady state before recording the pressure drops.
8. At the end of the experiment, stop water & air flow.
Formulae:
Where,
A
C
= Cross-sectional area of
the column
D
C
= Diameter of the column
F
L
= Flow rate of water
F
G
= Flow rate of air
L = Superficial mass velocity
of water
G = Superficial mass velocity
of air

w
= Density of water

a
= Density of air
R
1
= Manometer difference of water across the packed bed column
R
2
= Manometer difference of air in orifice meter
g = Acceleration due to gravity
P = Pressure drop
Z = Height of column between manometer taps

m
= Density of mercury/carbon tetrachloride.
3
( )
1
1
]
1

,
_

1
1
]
1

,
_

2
2
2
1
2
2
2
1
) ( 2
1
) ( 2
*
100
sec . /
sec . /
4
p
O
a
a w
O O
O
O O G
a m
C
a G
C
W L
C C
A
A
R
A C
A
A
P
A C F
g
R
P
m kg
A
F
G
m kg
A
F
L
D A

A
C
= 1.96 x 10
-3
Z = 50 cm
D
C
= 50 mm
O
C
= 0.61
A
O
=
2
4
O
D

A
P
=
2
4
P
D

Orifice meter diameter D

0
= 19 mm
Orifice pipe diameter D
P
= 38 mm
Rasching ring outer diameter 12mm
Density of mercury = 13.6 gm/cm3
Density of air = 1.2 x 10
-3
gm/ cm
3
Density of water = 1 gm/ cm
3
Observation table:
S.No Flow rate
of water
Manometer
difference
of air in
orifice
meter (R
2
)
Manometer
difference
Across the
column(R
1
)
Flow rate
of air
L
sec . /
2
m kg
G
sec . /
2
m kg
sec . /
2
m kg
4
Z
P
Result:
A hydrodynamics study in packed column is studied i.e. Vs. superficial velocity of gas
at various constant liquid velocities is plotted. Also compared with the literature data for
given system.
Analysis:
1. If the column leads to loading condition, mass transfer between the phases is very
low because of poor contact between the phases.
2. If the column leads to condition of flooding, the liquid particles are carried away by
gas molecules; mass transfer between the phases is very low.
3. The packed column may be used as absorption column or extraction column.
4. If pressure drop in the column is high, power consumption in the pump and blower
are high, ultimately it leads to high cost.
5. Optimizing the liquid flow rate and gas flow rate are in such a way that flooding
condition and loading conditions should not occur.
Applications:
1. It is especially used in vacuum distillation.
2. It is used for recover CO
2
air mixture by using water as a solvent.
3. It is used to recover SO
2
from SO
2
air mixture by using water as a solvent.
4. It is used in the separation of ammonia from ammonia air mixture by using water as
a solvent.
5. It is used to recover H
2
S form gas petroleum distillation by using triethanol amine
as solvent.
6. It is used to recover acetone from acetone air mixture by using water as a solvent.
In generally it is used in petrochemical nuclear and pharmaceutical industries.
5
Z
P
Precautions:
1. Pressure should be measured only after steady state is achieved. Otherwise
inaccurate results are obtained.
2. Regularly ensure that feed tank is filled with make up water.
3. Outlet of the packed column should be opened before doing the experiment.
Otherwise water will enter into the blower.
4. Vent off should be closed during the operation. Otherwise air may not enter into the
packed column.
5. Make sure that U-tube manometer limbs should be equal before doing the
experiment
Viva-voice questions:
1) Define operating holdup and static holdup?
2) What is flooding velocity when referred to packed towers?
3) What type of packing materials are used in the packed column?
4) How the size of the packing materials influence hold up?
5) Why it is necessary to study hold up in packed columns?
6
2. OPEN PAN EVAPORATOR
AIM: To find vaporization efficiency of an open pan evaporator & to calculate the heat
transfer coefficient
OBJECTIVE:
To study the concept of evaporation and to find the rate of heat transfer in an open
pan evaporator
SCOPE TO LEARN THROUGH EXPERIMENT:
1. To study simultaneous mass transfer and heat transfer
2. To compare evaporation concept with drying concept
3. To know the method of operation
THEORY:
Evaporation is a unit operation where in the solution is concentrated
by removal of solvent, namely water. It differs from drying in that the end product is a
solid rather than a liquid. It differs from distillation in that the end product is
concentrated solution rather than a vapor. When a liquid surface is open to atmosphere,
concentration gradient is set in between the liquid surface and atmospheric air. At the
liquid surface, the partial pressure of vapor will be equal to vapor pressure of liquid at
the surface temperature; the partial pressure of the vapor away from the liquid surface
is determined by water vapor present in the atmosphere. The performance of any
evaporator is governed by two factors, Capacity and Economy. Capacity is defined as
the amount of water evaporated /hr. Economy is the amount of water evaporated /kg of
steam.
*Steam consumption is defined as
Capacity/Economy.
*The vaporization efficiency is defined as
Heat supplied per evaporating a fixed amount of water/
Theoretical amount of heat required.
7
EQUIPMENT USED:
Steam heated boiler and pan
SPECIFICATIONS:
Diameter of open pan = 40 cm
Height of open pan = 8 cm
Steam boiler capacity = 40,000 cm3
MATERIALS USED: Water / Milk
EXPERIMENTAL PROCEDURE:
1. The diameter of the vessel is measured.
2. Steam boiler is started and pressure is allowed to build.
3. 1 litre of water is measured and poured into the pan
4. Steam is allowed to flow, by opening the valve and steam pressure is adjusted to
(0.5 to 1.0 kg/cm
2
). Stop clock is started.
5. The evaporation is continued till 75% of the liquid is evaporated.
6. The boiling temperature of water is noted down.
7. The condensate flow rate is measured.
8. Steam supply is stopped and boiler is switched off.
OBSERVATIONS:
8
Pan
Condensate
Outlet valve
Steam
Jacket
Boiler
Pressure Gauge
Open Pan Evaporator
Initial weight of water = W1 kg
Final weight of water = W2 kg
Pressure gauge reading = kg/cm
2
,
Inlet temperature of steam, T
S
= C
Initial temperature of water = Tw1 C
Final temperature of water = Tw2 C
Total time of evaporation, t = min
Mass of steam condensate collected, m = kg
CALCULATIONS:
Amount of water evaporated, V = W1-W2
Rate of evaporation, V
1
= V/t kg/min
Rate of heat transfer = V
1
* J/min,
where = Latent heat of vaporization at atm. pressure
Steam rate, m
1
= m/t
Vaporization efficiency = (V
1
/m
1
) *100
Heat transfer area == * (1.2d)
2
/4 m
2
Average water boiling temperature = (Tw1+Tw2)/2 =Tw
Q =UAT
U = Q/ (A* (Ts-Tw)) W/m
2
C
RESULTS:
Vaporization efficiency =
(Range = 30 % to 40 %)
Heat transfer coefficient =
(Range = 4000 to 4500 J/m
2
minC)
ANALYSIS:
1. Compare the value of vaporization efficiency obtained with the actual value.
2. Compare the value of Heat transfer coefficient obtained with the actual value.
3. Study the simultaneous mass transfer and heat transfer taking place in the
evaporator
4. Compare evaporation concept with drying concept
9
5. Study the method of operation i.e. batch or continuous
APPLICATIONS:
1. Sugarcane processing
2. Production of sugar in the tropics by open pan evaporation processes
3. Recovery of sodium hydroxide in Kraft pulping
PRECAUTIONS:
1. Water should be filled to at least 50 % in the boiler, before switching on the two
heaters.
2. The pressure gage should be continuously monitored for increase in pressure due to
steam formation.
3. Care should be taken when measuring the condensate flow rate.
4. The inlet valve should be closed when steam outlet valve is opened for steam to
enter the pan.
5. The pan becomes very hot and shouldnt be touched with hands while measuring
the temperature.
VIVA-VOICE QUESTIONS:
1) What is difference between drying and evaporation?
2) What do you mean by overall heat transfer coefficient?
3) What do you mean by LMTD?
4) What do you mean by economy of an evaporator?
5) Define capacity of an evaporator?
6) On what factors heat transfer coefficient depends?
10
3. LIQUID LIQUID EXTRACTION
AIM: To obtain the equilibrium distribution data for ternary system and to obtain as
equation to fit in the data.
OBJECTIVES:
1. To understand the concept of Extraction.
2. To understand the concept of solubility.
Theory:
Liquid-liquid extraction or solvent extraction is the separation of the components of a
liquid solution by contact with another liquid solvent, which is relatively immiscible with
feed solution. The liquid, which is added to the solution to bring out extraction, is known
solvent. This solvent takes up part of the solute and forms an immiscible layer with
remaining solution. The solvent layer is called extract and the other layer is called raffinate.
The separation of aromatics from kerosene based fuel oils, the production of nuclear fuels
in the industry and the separation of penicillin from fermentation mixtures are examples of
application of solvent extraction method. Thus extraction process utilizes the difference in
solubility of components in the solution.
Extractions involves the use of systems composed of at least three substances and
although for the most part of the insoluble phases are chemically very different, generally
three components appear at least to some extent in both phases. Examples are Benzene (A),
Water (B) and acetic acid (C) etc. Liquid C dissolves completely in A and B but A and B
dissolve only to a limited extent in each other. In the above mentioned example, after some
time equilibrium is attained between the two layers that is one layer containing acetic acid
dissolved in water and in other layer, acetic acid is dissolved in benzene.
Apparatus:
Five 100 cc bottles with stoppers, five separating funnels, burette, conical flasks,
volumetric flasks, pipettes and weighing balance.
System:
Benzene, Water and Acetic acid.
Procedure:
1. Take five 100 cc bottles with stoppers and clean them well.
2. To each one of them add 25 cc of benzene and 25 cc of distilled water from
separate burette.
3. Add 1cc, 2cc, 5cc, 10cc, 15cc glacial acetic acid from a burette, in the 1
st
, 2
nd
,
3
rd
, 4
th
and 5
th
bottles respectively. Shake the bottles for an hour for the contents
11
to settle. Meanwhile prepare 3N sodium hydroxide solution and standardize
with standard oxalic acid with phenolphthalein as indicator.
4. After one hour, separate the two layers in each bottle with the help of 250cc
separating funnel.
5. Take 10ml of aqueous layer in conical flask and titrate against prepared sodium
hydroxide solution using phenolphthalein solution as indicator,
6. Find the amount of acetic acid present in aqueous layer. Repeat this procedure
for remaining aqueous solution layers.
* While titrating the organic layer initially, add about 10cc of distilled water.
7. Calculate the weight of acid in gm/100gm of each layer and tabulate the data.
8. Draw a graph between the concentration of the acid in organic against the
concentration of acid in aqueous on a graph. If it is curve, plot the data on log-
log graph sheet and obtain the equation, which fits the experimental data.
TABLE: 1
STANDARDISATION OF NaOH:
S.No Volume of Oxalic acid
(ml) V
1
Volume of NaOH Volume of NaOH
run down (ml) V
2 Initial (ml) Final (ml)

Normality of Oxalic acid, N
1
= 1N
(VN)
NaOH
= (VN)
Oxalic acid
i.e. V
1
N
1
= V
2
N
2
TABLE: 2
S.No Amount of acetic
acid added (ml)
Aqueous layer
(denser)
Organic layer (lighter)
Weight
( S x V)
Titre value
(ml)
Weight
( S x V)
Titre value
(ml)
12
Calculations:
Normality = No. of moles equivalent
Volume (liter)
No. of moles = Volume x N
= Titre value x N
Wt. of acetic acid = no of moles equivalent * equivalent weight
Weight fraction of acetic acid =
TABLE: 3
S.No Volume of
acetic
acid added
(ml)
Aqueous layer
(denser)
Organic layer
(lighter)
Wt. of
acetic acid
Wt.
fraction
Wt. of
acetic acid
Wt.
fraction
Result: The equilibrium equation obtained from experiment is y = m x
n
ANALYSIS:
1. Study the temperature effect on extraction.
2. Study the solubility concept.
APPLICATIONS:
Extraction processes are well suited to the petroleum industry because of the need
to separate heat sensitive liquid feeds according to chemical type (e.g. aliphatic, aromatic,
naphthalene rather than by molecular weight or vapor pressure.
Other major applications exist in the biochemical or pharmaceutical industry, where
emphasis is on the separation of antibiotics and protein recovery. In the inorganic
13
component such as phosphoric acid, boric acid & sodium hydroxide from aqueous
solutions. Some examples are given below.
1. Extraction of Nitrobenzene form after reaction of HNO
3
with toluene in H
2
SO
4
.
2. Extraction of methyl acrylate from organic solution with perchloroethylene.
3. Extraction of caprolactum from ammonium sulphate solution with benzene.
4. Extraction of acrylic acid from waste water with butanol.
5. extraction of methanol from LPG with water
6. Extraction of chloroacetic acid from methylchloroacetate with water.
7. Removal of a component present in small concentration.
Example: hormones in animal oil.
8. Recovery of heat sensitive materials, where low to moderate processing
temperatures are needed
PRECAUTIONS:
1. Add same quantity of indicator to all samples to be analyzed while doing the
experiment
2. Care must be taken while handling the chemicals.
3. Lid in separating funnel should be removed while separate the organic layer and
aqueous layer.
4. Ensure that there are no spherical drops in both aqueous layer and organic layer
before separating both layers.
VIVA-VOICE QUESTIONS:
1. What is the extraction?
2. What is the difference between liquid extraction and leaching?
3. What is the temperature effect on extraction?
4. Analyze the nature of the given system.
5. What is the pressure effect on extraction?
14
4. SOLID-LIQUID EQUILIBRIUM
AIM: To verify the Freudlich equation by Adsorption of Oxalic / Acetic acid on activated
carbon from oxalic / acetic acid solution & to calculate the constants of equation.
OBJECTIVES: To know the concept of adsorption of a weak acid on activated carbon and
to study the validity of the Freundlich adsorption isotherm.
SCOPE TO LEARN THROUGH EXPERIMENT:
1. To know the types of adsorption i.e. physical or chemical
2. To know the nature of adsorbents depending on surface area
3. To know the method of operation

THEORY:
One of the operations where solid liquid equilibrium is used is adsorption. These
adsorption operations exploit the ability of certain solids preferentially to concentrate
specific substances from solutions onto their surfaces. In these operations the mixture to be
separated is brought into the contact with another insoluble phase, the adsorbing solid and
the unequal distribution of the original constituents between the solid surface and the bulk
of the fluid permits a separation to be made. In this the solid is known as adsorbent and the
component adsorbed is known as adsorbate.
Formula used: Freundlich adsorption isotherm: - (for dilute solutions)
At a given temperature,
Mass of a solute adsorbed by a solid adsorbent at various amounts is given by the
following empirical relation.
C* = K [V (C
0
C*)]
n
Where C
0
= initial concentration of Oxalic acid solution
C* = equilibrium concentration after adsorption
V = Volume of given solution / mass of solid
K, n are constants at a given temperature for a given solute and adsorbent.
System: Activated charcoal, water and acetic acid.
Apparatus used: Five bottles with stopper, conical flask, burette with stand, funnel,
pipette, measuring jar.
PROCEDURE:
15
1. Prepare 250 ml of 0.1 N NaOH solution.
2. Prepare 250 ml of 0.1 N Oxalic acid for standardization of NaOH solution.
3. Take 5 reagent bottles and label them 1 to 5.
4. Take 5 grams of charcoal in each flask, and add 100cc of distilled water.
5. Add 1ml, 5ml, 10ml, 15ml and 20 ml of acetic acid in the flasks.
6. Close the lids and keep the bottles in a shaker. Switch on the shaker and operate
it for about 30 minutes, at which time the equilibrium is expected to reach
between the liquid and solid phases.
7. Remove the bottles from the shaker; filter the contents of each bottle using
normal filter paper.
8. Collect the clear solution in 5 separate 250ml conical flasks also numbered 1 to
5.
9. From each of these solutions take 10 ml with pipette and titrate against the
standardized NaOH solution using phenolphthalein indicator.
A plot of X Vs Y is drawn which shows the equilibrium distribution data for the
given system.
Standardization of NaOH:
S.No Volume of Oxalic acid
(ml)
Volume of NaOH (ml) Volume of
NaOH run down
(ml)
Initial Final
Normality of Oxalic acid = 1N
Volume of Oxalic acid = 10ml
Volume of NaOH = _____ ml
Normality of NaOH = _____
(VN)
NaOH
= (VN)
Oxalic acid
Normality of NaOH =
OBSERVATIONS:
16
S.No Volume
of
Sample
(ml)
Volume of
Acetic acid
(ml)
Volume of
NaOH run
down (ml)
Normality
of sample
Wt. of acetic
acid in
aqueous
layer
Wt. of
acetic
acid in
feed
Wt. of
acetic
acid in
charcoal

Calculations:
Normality =
Weight of acetic acid in aqueous layer =
Weight of acetic acid in feed = Volume * Density of acetic acid
Amount of acetic acid in charcoal = Weight of acetic acid in feed - Wt. of acetic acid in
aqueous layer
DATA ANALYSIS:
Normality of Acetic acid, N
0
=
Normality of the bottle 1 filtrate, N
1
= (Normality of NaOH x burette reading) / 10
Initial concentration of Acetic acid,
C
0
= N
0
x equivalent weight of Acetic acid, Kg acid / m
3
solution
Equilibrium concentrations of filtrate after adsorption,
C* = N1 x equivalent weight of Acetic acid, Kg acid / m
3
solution
V = Volume of Acetic acid
Weight of adsorbent
Bottl
e No.
Weight
of
adsorben
t, gm
Volume
of
Acetic
acid, ml
V,
m
3
/ Kg
C* ,
Kg / m
3
log C*
V( C
0

C*)
log[V
(C
0
-C*)]
1 5 1
2 5 5
3 5 10
4 5 15
5 5 20
GRAPH: -
The Freundlich adsorption isotherm over the small concentration range is
C* = K [ V( C
0
C* ) ]
n
17

log C* = log K + n log [ V( C
0
C* ) ]

Plot a graph between log C* Vs log [V (C
0
-C*)]. A straight line is drawn fitting all the
five points. Calculate the slope (n) and intercept (log k).
RESULT:
1. A straight line obtained in the plot shows the validity of the Freundlich adsorption
isotherm over the concentration range studied.
2. The values of n and K are ____________&_____________
ANALYSIS:
1. Study the method of operation i.e. batch or continuous
2. Study the temperature effect on adsorption
3. Study the pressure effect on adsorption
4. Compare solid-liquid extraction with liquid-liquid extraction
5. Study the types of adsorption i.e. physical or chemical
6. Study the nature of adsorbents depending on surface area
APPLICATIONS:
Liquid Purification:
1. Removal of H
2
O from organic solutions
2. Removal of organics from H
2
O
3. Removal of sulfur compounds from organic solutions.
4. Decolorization of solutions
Liquid bulk separation:
1. Normal paraffins / iso-paraffins
2. Normal paraffins / olefins
3. P xylene / other C8 aromatics
4. P or m cymene / other cymene isomers
5. Fructose / dextrose, polysaccharides.
PRECAUTIONS:
Distilled water should be added in exactly measured quantities.
Calibration chart should be prepared with utmost accuracy.
18
VIVA-VOICE QUESTIONS:
1) What is the difference between adsorption and absorption?
2) What are the types of adsorptions?
3) What is Freundlichs equation?
4) What is Langmuirs equation?
5) What is Adsorption Isotherm?
19
5. LEACHING
AIM: To determine the solid-liquid equilibrium data for the given leaching system and
represent it in the form of Nx vs X and Ny vs Y graphs
OBJECTIVE: To know the concept of leaching & to find the relationship between
concentration of solid and weight fraction of solute.
SCOPE TO LEARN THROUGH EXPERIMENT:
1. To know the method of operation i.e. batch or continuous
2. To compare leaching with liquid-liquid extraction
3. To study the preparation of solid (coarse grains/fines)
PRINCIPLE: Removal of materials by dissolving them away from solids is called
Leaching. The chemical process industries use leaching but the process is usually called
extraction, and organic solvents are often used.
FORMULA USED:
Weight fraction of NaCl in liquid phase = X= [C/ (A+C)]
liquid
Concentration of sand in liquid phase= Nx= [B/ (A+C)]
liquid
Weight fraction of NaCl in solid phase= Y=[C/ (A+C)]
solid
Concentration of sand

in solid phase=N
Y
= [B/ (A+C)]
solid
S.G sample = [weight of S.G bottle with sample]-[weight of empty S.G. bottle]
[Weight of S.G. bottle with distilled water]-[weight of empty S.G. bottle]
Notation Scheme adopted:

A: water (wt)
B: sand/CaCO
3
(wt)
C: NaCl (wt)
APPARATUS USED:
250 ml beakers-5, 100ml measuring jar, glass rod, specific
gravity bottle, Electronic weighing balance.

MATERIALS USED:
NaCl, sand / CaCO
3,
Water
20
EXPERIMENTAL PROCEDURE:
1. Take five 250ml beakers.
2. Take 20gms of CaCo
3
(or sand) in each beaker.
3. To each beaker add 5, 10, 15, 20, 25gms of NaCl. Mix thoroughly with a glass rod.
4. See that there are no lumps inside.
5. Add 100ml of distilled water to each beaker. Mix thoroughly with a glass rod.
6. Allow the contents of the 5 beakers to settle say for 1 hour.
7. During this time prepare the calibration chart.
8. Separate the liquid phase from solid phase. (decant) (Pipette may be used).
9. Measure the volume of the clear liquid. Measurement should be done without error.
10. Find the specific gravity of the clear liquid from each beaker by the specific gravity
bottle method.
OBSERVATIONS:
Observation Table 1:
S.No. Beaker No. Wt. of sand(or
CaCO
3
) taken
(gms)
Wt of NaCl
taken (gms)
Distilled
water added
in ml
Volume of
separated
clear
solution (ml)
1 1 20 5 100
2 2 20 10 100
3 3 20 15 100
4 4 20 20 100
5 5 20 25 100
Observation Table 2:
21
S.No. S.G. of clear solution
1
2
3
4
5
DATA ANALYSIS:
Preparation of Calibration Chart:
Prepare NaCl-Water solutions of varied concentrations as shown in the table below and
Find specific gravity by bottle method. Tabulate the results as shown below.
Calibration chart is prepared by plotting a graph between NaCl concentration on X axis
and S.G. of sample on Y axis.
S.No Water (gm) NaCl (gm) Wt%
(NaCl
concentration)
S.G. of
sample
1 95 5 5
2 90 10 10
3 85 15 15
4 80 20 20
5 75 25 25
Calculations Table:
S.No Beaker No. X Y Nx N
Y
1 1
2 2
3 3
4 4
5 5
Calibration chart preparation:
1. A calibration graph Wt% of NaCl Vs specific gravity of sample
2. Plot Nx Vs X and N
Y
Vs Y in the same quadrant. Take Nx , N
Y
on Y-axis and X , Y
on X-axis
RESULT:
Equilibrium data is represented as a graph between Nx vs X and N
Y
vs Y
22
ANALYSIS:
1. Study the method of operation i.e. batch or continuous
2. Study the temperature effect on leaching
3. Compare leaching with liquid-liquid extraction
4. Study the preparation of solid (coarse grains/fines)
APPLICATIONS:
1. Sulfuric acid leaching of nickel and cobalt from ores.
2. Oxidation of pyrite, followed by cyanide leaching of precious metals under
ambient conditions.
3. Leaching is a widely used extractive metallurgy technique which converts metals
into soluble salts in aqueous media.
PRECAUTIONS:
The specific gravity bottle should be thoroughly cleaned and weighed.
Distilled water should be added in exactly measured quantities.
Calibration chart should be prepared with utmost accuracy.
VIVA-VOICE QUESTIONS:
1. What is leaching?
2. What are the applications of leaching?
3. What is difference between leaching and liquid extraction?
4. What is the temperature effect on leaching?
6. TERNARY LIQUID EQUILIBRIUM
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AIM: To obtain the solubility characteristic curve of a given liquid liquid system by
plotting on a triangular graph or rectangular graph.
OBJECTIVE: To know the concept of Extraction.
SCOPE TO LEARN THROUGH EXPERIMENT:
1. To know the solubility concept.
2. To plot the bimodal solubility curve, and find the plait point.
THEORY:
Liquid extraction sometimes called solvent extraction is the separation of the
constituents of a liquid solution by contact with another insoluble liquid, if the substances
containing the original solution distribute themselves differently between the two liquid
phases, certain degree of separation will result and this can be enhanced by use of multiple
contacts.
Extraction involves the use of systems composed of at least three substances and
although for the most part of the insoluble phases are chemically inert very different,
generally all three components appear at least to some extent in both phases.
A three liquid system with one pair partially soluble is the common type of system
in extraction and typical examples are water (A), Chloroform (B), Acetone (C), liquid C
dissolves completed in A & B but A & B dissolve only to limited extent in each other.
System: Benzene, Water and Acetic acid.
Apparatus used: 50 ml burettes-3, 250 ml conical flask, 250 ml beakers-2, 10 ml pipette
PROCEDURE:
1. Take 10ml of benzene is in a 100ml stopper bottle.
2. Titrated with water with the help of micro burette.
3. Take 9ml of benzene and 1ml of acetic acid mixture into another bottle and
titrate with water.
4. The procedure is repeated for 8ml of benzene and 2ml of acetic acid and so on
until 10ml of pure acetic acid.
5. The titre values are noted down.
6. In the record step, 0 ml acetic acid and 10ml of water are taken in a bottle and is
titrated against benzene. The end point is turbidity of the solution.
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7. Again 1ml of acetic acid and 9ml of water is taken and is titrated against
benzene. The procedure is repeated for 2ml of acetic acid and 8ml of water and
so on until 10ml of acetic acid and water. The titre values are noted down.
Plot the wt fraction calculated in part I and Part II on a triangular chart.
OBSERVATIONS:
Table -1:
S.No. Vol. of
Benzene(ml)
Vol. of acetic
acid (ml)
Vol. of distilled
water (ml)
1. 10 0
2. 9 1
3. 8 2
4. 7 3
5. 6 4
6. 5 5
7. 4 6
8. 3 7
9. 2 8
10. 1 9
11. 0 10
TABLE -2:
S.No. Vol. of distilled
water (ml)
Vol. of
Acetic acid
(ml)
Vol. of Benzene
(ml)
1. 10 0
2. 9 1
3. 8 2
4. 7 3
5. 6 4
6. 5 5
7. 4 6
8. 3 7
9. 2 8
10. 1 9
11. 0 10
S.No Part I Part II
Y
A
Y
B
Y
C
X
A
X
B
X
C
1
2
25
3
4
5
6
7
8
9
10
CALCULATIONS:
Density
Y
A
= Weight fraction of water in part I
Y
B
= Weight fraction of benzene in part I
Y
C
= Weight fraction of acetic acid in part I
X
A
, X
B
, X
C
are mass fractions of water, benzene and acetic acid respectively in part II.
Density of water (A) = 1 g/cc
Density of Benzene (B) = 0.79 g/cc
Density of Acetic acid (C) = 1.049 g/cc
RESULT: The binodal solubility curve is plotted on the triangular graph and Plait point is
determined.
ANALYSIS:
1. Study the solubility concept.
2. Compare the plotted solubility curve with the literature.
3. Compare the plait point with the literature.
APPLICATIONS:
Extraction processes are well suited to the petroleum industry because of the need
to separate heat sensitive liquid feeds according to chemical type (e.g. aliphatic, aromatic,
naphthalene rather than by molecular weight or vapor pressure.
Other major applications exist in the biochemical or pharmaceutical industry, where
emphasis is on the separation of antibiotics and protein recovery. In the inorganic
component such as phosphoric acid, boric acid & sodium hydroxide from aqueous
solutions. Some examples are given below.
1. Extraction of Nitrobenzene form after reaction of HNO
3
with toluene in H
2
SO
4
.
2. Extraction of methyl acrylate from organic solution with perchloroethylene.
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3. Extraction of caprolactum from ammonium sulphate solution with benzene.
4. Extraction of acrylic acid from waste water with butanol.
5. extraction of methanol from LPG with water
6. Extraction of chloroacetic acid from methylchloroacetate with water.
7. Removal of a component present in small concentration.
8. Example: hormones in animal oil.
9. Recovery of heat sensitive materials, where low to moderate processing
temperatures are needed
PRECAUTIONS:
1. Care must be taken while handling the chemicals.
2. Do not pipette out the acetic acid from bottle.
3. Same amount of indicator should be added each time and the readings are noted
carefully
4. Care must be taken in adding 1ml of content.
VIVA-VOICE QUESTIONS:
1) What is the nature of the system?.
2) What is tie line?
3) What is binodal solubility curve?
4) What is the effect of pressure and temperature on solubility?
5) How a ternary system is plotted on a triangular graph sheet?
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