SUBMITTED TO:

Sir Rizwan
Ali

Separation
SUBMITTED BY:
Processes
2013-CH-50
2013-CH-52
2013-CH-78
2013-CH-80
2013-CH-94

LAB LAYOUT

LIST OF EQUIPMENT

1) Ion Exchange Apparatus

2) Gaseous Diffusion Apparatus
3) Old Distillation Column
4) Continuous Distillation column
5) Batch Distillation Column
6) Liquid/Liquid Extraction Unit
7) Gas/Liquid Extraction Unit
8) Tray Drier
9) Fluid Bed Drier

EQUIPMENT DETAILS
CONTINUOUS DISTILLATION COLUMN
Continuous distillation column is used to demonstrate the working of a
continuous distillation. It is also used to perform azeotropic distillation.

BATCH DISTILLATION COLUMN

Similarly the batch distillation column in construction (with the exception of
reboiler), is used to demonstrate the batch distillation process at constant
reflux ratio and at constant product composition. The effect of process
variables(like reflux ratio) are also studied.

LIQUID/LIQUID EXTRACTION COLUMN

Packed column for liquid, liquid extraction is used for calculation of
coefficient of distribution for liquid-liquid extraction. First of all the solute is
extracted from the feed using an appropriate solvent. Then for separation
distillation system is equipped with column.

GAS/LIQUID ABSORPTION COLUMN

The absorption column is used to demonstrate the problems of packed
column such as flooding, channeling and entrainment. We can also measure
the chemi-sorption equilibrium using a gravimetric analysis.

GASEOUS DIFFUSION APPARATUS

This apparatus is used to measure the diffusivity of a volatile component at a
controlled temperature.

TRAY DRIER

Try drier is used for the study of drier and understand the theoretical
fundamentals like drying curve, effect of temperature and air velocity on the
drying rate, etc.

FLUID BED DRIER

The exposed surface of wet particles can be greatly enhanced by fluidizing
the solid particles, therefore the rate of drying increases significantly. This
lab-scale equipment is used to demonstrate the fluid bed drying principle.

ION-EXCHANGE APPARATUS
Water softening and several other industrial operations make use of the ion
exchange process. The apparatus is used forthe demonstration of cationic
and anionic resins for this purpose, to measure the exchange capacity,
normal operation and regeneration of the ion-exchange system.

SAFETY RULES

Follow all the instructions carefully. If you do not understand a

direction or part of a procedure, ask your teacher before proceeding
with the
Manual should be read before taking any reading (or step) in the
laboratory
Do not work alone in the laboratory. Always understand the teachers
instruction first then start your experiment
Unauthorized experiments are not allowed. Perform only those
experiments authorized by your teacher
Do not touch any equipment, chemicals, or other materials in the
laboratory area until you are instructed to do so
Do not eat or drink anything in the laboratory
Always work in a well-ventilated area
Work areas should be kept clean and tidy at all times.
Equipment of lab are very expensive, so they should be handle with
great care and must be used under the supervision of teacher or in
presence of lab attendant
SOPs of the equipment must be followed

THEORY OF DISTILLATION
Distillation is one of the most common liquid-liquid separation processes, and
can be carried out in a continuous or batch system.
Distillation works by the application and removal of heat to exploit
differences in relative volatility. The heat causes components with lower
boiling points and higher volatility to be vaporized, leaving less volatile
components as liquids. Mixtures with high relative volatilities are easier to
separate. This makes separations of close-boiling and azeotropic feeds
difficult, so special distillation techniques have to be used to separate these
mixtures.
Distillation can be used to separate binary or multi-component mixtures.
Many variables, such as column pressure, temperature, size, and diameter
are determined by the properties of the feed and the desired products. Some
specialized columns perform other functions, such as reactive distillation
columns, which combine reaction and separation of products into a single
unit.
The feed enters a plate column towards the middle of the column.
Concentration differences cause the less volatile components to transfer
from the vapor stream to the liquid stream. The vapor exiting the condenser
contains the most volatile components, while the least volatile components
exit
through
the
reboiler
in
the
liquid
stream.
SIEVE PLATE
The plate or tray column is the most widely used type of distillation column.
The number of trays or stages in the column is dependent on the desired
purity and difficulty of separation. The number of stages also determines the
height of the column. In the laboratory 8 plates are used.

APPLICATIONS
The application of distillation can roughly be divided in four groups:
laboratory scale, industrial distillation, distillation of herbs for perfumery and
medicinal (herbal distillate) and food processing. The latter two are distinct
from the former two, in that in the distillation is not used as a true

purification method, but more to transfer all volatiles from the source
materials to the distillate.

The main difference between laboratory scale distillation and industrial

distillation is that laboratory scale distillation is often performed batch-wise,
whereas industrial distillation often occurs continuously. In batch distillation,
the composition of the source material, the vapors of the distilling
compounds and the distillate change during the distillation. In batch
distillation, a still is charged (supplied) with a batch of feed mixture, which is
then separated into its component fractions which are collected sequentially
from most volatile to less volatile, with the bottoms (remaining least or nonvolatile fraction) removed at the end. The still can then be recharged and the
process repeated.

In continuous distillation, the source materials, vapors and distillate are kept
at a constant composition by carefully replenishing the source material and
removing fractions from both vapor and liquid in the system. This results in a
better control of the separation process.

EXPERIMENT NO: 1
OBJECTIVE
Use of the refractometer to determine mixture compositions.

EQUIPMENT SETUP
Throughout the experimental procedures carried out on the Continuous
Distillation Column, it I essential to have convenient quick method of
determining the composition of the binary mixture taken from the various
samples on the equipment. Such a method involves the use of refractometer.
Since the refractive index of these mixtures varies with compositions. The
only equipment needed in addition to the hand held refractometer is a
measuring cylinder 0-100 ml, a suitable container to mix the sample in a
bottle of each of the pure component of the binary mixture to analyze.

SUMMARY OF THEORY
For the system, water/ethanol mixture, of the known concentration can be
made up and their refractive indexes can be measured. The refractometer
measures the critical angle of the liquid under test and each concentration
will show a different critical angle.
= Critical Angle

Beyond the critical angle is darkness and refractometer are calibrated along
this light/dark boundary.

PROCEDURE
Measure the refractive index (RI) of pure water and pure ethanol.
For 25 mole percent ethanol i.e. 75 mole percent water.
Molecular weight of water = 18
Molecular weight of ethanol = 46
Density of water = 1 g/mL
Density of ethanol = 0.789 g/mL
For calculation purposes,

Chemical E = Ethanol
Chemical W = Water

After simplifying, the final expression is,

Volume (Total) = 3 0.62 Volume (Ethanol)
Volume (Total) = 1.86 Volume (Ethanol)
Thus for 100 mL of mixture, quantities required will be
Ethanol = 53.76
Water
= 46.24

EXPERIMENT NO: 2
OBJECTIVE
To study the pressure drop across the column against various boil-up rates

THEORY
The pressure drop across the column is the sum of the resistance offered to
the vapors by the sieves tray and the resistance offered by the liquids to the
vapors to pass through them.
The vapor velocity is directly related to the pressure drop. As the velocity is
increased, pressure drop across the column increases. Vapor velocity is
controlled by the power input to the boiler so as the power input increases
vapor velocity increases. Thus increasing the boil up rate will increase the
pressure drop across the column
When no liquid is present these sieve behaves as orifice and pressure drop is
directly proportional to square of velocity. When liquid is present the vapors
have to overcome the liquid head. So the relation will change. in the log-log
graph of pressure drop against boil-up rates first it will be constant and then
after foaming a large pressure drop will exist. A small change in boil-up rate
will cause large pressure drop.

EQUIPMENT SET-UP
The equipment will be setup to operate at total reflux. All vapor will be
condensed to liquid and return to column. No top or bottom product will be
obtained and feed is once charged in the reboiler through the filler cap. To
calculate the boil-up rates a measuring cylinder and stop watch is also
required.

PROCEDURE
Before starting the experiment close all the valves except V10 for the reflux.
Open the filler cap of the boiler and fill 10 liters of the solution in boiler and
close the boiler filler cap properly. Now open the water valve for the

condenser V5. Now set the temperature knob on T9 showing the

temperature of the reboiler on the controller screen. Then turn on the boiler
and set the power to 0.75 kW. The boiler will start to heat up the liquid. Open
the valves of the column connected to the manometer, V6 & V7. Initially
there will be no pressure difference so there will be no readings. Close the
valves.
After sometime temp of the column will start increasing and vapor will move
up to the condenser. After condenser liquid will move in the distillate vessel
and move in the valve (which is switched off). Now as we are operating the
column on total reflux so all the liquid will move back to the column. This
valve is switched on from the controller.
The liquid will then cascade down forming a level on the trays. Bubbles will
pass through the liquid and the system will achieve an equilibrium position
when the temperature on the trays i.e. from T1 to T8 becomes constant.
To calculate the boil up rate valve V3 is opened and sample is taken in a
measuring cylinder and the time is recorded. One precaution is very
important while measuring the boil up rate. Before starting to collect in a
measuring cylinder, liquid from the pipe should be poured in separate flask
and when liquid is flowing steadily in the pipe, the measure the boil up rate
(liquid in measuring cylinder in a recorded time).
After calculating the boil up rate pressure drop is calculated by open both the
valves V6 & V7. It must be kept in mind that V6 should be opened first then
V7 and while closing the valves after measuring the pressure drop V6 must
be closed first and then V7. This order is followed to prevent the vapors
entering into the manometer from column. Repeat the reading until two in a
row are fairly close.
Repeat the same procedure for different boil up rates. Give a time of 5-10
minutes to achieve steady state in the column. Using an increment of 250
watt take readings up to 1.5kW.

EXPERIMENT NO: 03
OBJECTIVE
To determine overall efficiency of column at varying boil-up rates

THEORY
To calculate theoretical number of plates for a given separation at total reflux

FENSKES METHOD

n+1=
Where

/ log[b]av

n = Number of theoretical plates

xa= mole fraction of more volatile component
xb = mole fraction of least volatile component
aav = average relative volatility
Subscripts D and B represents distillate and bottom respectively
b = [b.d]

The efficiency is given by

E=

* 1OO %

Knowing the composition of distillate and bottom and the corresponding

volatilities, the column efficiency can be easily determined.

EQUIPMENT SETUP

The equipment is setup to operate at the total reflux so the charge of the
feed mixture can be directly loaded in the reboiler by the feed cap provided
without first charging of the feed tanks. At total reflux there will be no feed or
top product or bottom products.
Make 1O liters of the mixture of water and ethanol with 5O% mole percent of
both. Required volumes for the mixture are
Water = 4.89 liters
Ethanol = 5.11 liters
We also require

25O ML measuring cylinder

Stop watch
Hand held refractor

PROCEDURE
Start the apparatus and fill the reboiler with 1O liters of the mixture. Set the
heat controller high at first, then reduce the heat as reflux is introduced to
give steady bubbling at all tray and total reflux. Leave the system for at least
3O minutes so that system can reach at the equilibrium state.
Measure the boil up rate as described in experiment A using valve V3. Do
this three times and use an average values. Take a sample of the overheads
from the valve V3. When doing that, be careful never to drain the
condensate reflux line i.e. partially open the valve V3 to leave the liquid in
the line all the time.
Generally, while taking samples, drain a discarding sample of
approximately 5 to 1O ml before taking the representative sample in small
glass. Do not drain too much of the discarding sample because of the
disturbance of mass balance. Discard the discarding sample in a safe way.
After the representative sample has been taken, keep the representative
sample in the upright position so there is no human error or minimum human
error is involved in the experiment. Sample can be easily evaporated so do
not over turn the samples as well.
Record the refractive index for the overhead sample. Similarly take a sample
of the bottom products using the valve V2. Be careful as this sample is hot.
Note the refractive index for this sample too.

Repeat this procedure every ten minutes until five samples for both bottom
and top products is obtained. We can calculate the temperature of the
column by simple taking the readings from temperature sensors T1 and T8.
Repeat this procedure for several different boil-up rates to cover over the
range of the column. The calibration graph developed can be used to
determine the concentrations of the components of the samples.