DISTILLATION COLUMN

Objective :
1) To determine the number of theoretical
plates at total reflux.

List of Equations:
 LIST OF EQUATIONS
• Weight of ethanol g =amount of ethanol mL ×density
kgm3
• Weight of water g =amount of water mL ×density
(kgmL)
• Weight percent of ethanol =weight of ethanol/(weight
of ethanol+weight of water) ×100%
• Mole of ethanol mol =weight of ethanol (kg)/molecular
weight (kgmol )
• Mole of water mol =weight of water (kg)/molecular
weight (kgmol )
• Mole percent of ethanol=mole of ethanol /(mole of
ethanol+mole of water )×100%
 PROCEDURE
• General startup Procedure
1. Make sure all the valves are closed
2. Turn on the power for the control panel
3. Make sure that 20L of a mixture of water and ethanol
already in the reboiler
4. The reflux divider (KFS-101) was set to total reflux
which is no. 2.
5. Let the cooling water flows into the condenser.
6. The cartridge heaters was switched on and allowing
the ethanol solution to boil.
7. Let the distillation column to stabilize.
• Continuous Process Procedure
1. 1. The system was allowed to be stabilized at temperature
approximately 0.2 .C.
2. The pump P1 was turned on and valve V2 was opened.
3. The reflux ratio was set to 1:1 (No. 3) and constant
throughout the process.
4. The heater W5 was turned on to preheated the feed of
ethanol-water to desired temperature which is 25 .C.
5. Valve V7 was opened partially to let the flow out of the
system.
6. The system was let until the inlet temperature are constant
at desired temperature.
7. Sampling Procedure was conducted.
8. The Process was repeated with different inlet temperature
which is 27 ⁰C.
• Sampling Procedure
Distillate sampling:
1. The remaining liquid in the sampling valve V11
was drained.
2. A vial was placed below valve V11.
3. The reflux divider (KSF-101) was set to distillate
off take (No. 1) for a few seconds.
4. Valve V11 was opened and 5-10 ml of samples
was collected and the valve was closed.
5. The reflux divider was switched back to original
setting (No. 3).
Bottom sampling:
1. Stagnated liquid remain in the valve V8 was
drained.
2. A vial was placed below valve V8.
3. Valve V8 was fully opened and V7 was partially
opened, 5-10 ml samples were collected and both
valves are closed.
4. The samples was cooling before analyzed.
Composition Analysis of Ethanol in Concentrated
samples procedure.
1. 10 ml of measuring cylinder was placed on a weighing
scale and the scale was set to zero.
2. By using a dropper, 1 to 2 g of samples were
transferred into the measuring cylinder and the sample
weight was recorded.
3. Water was added into the measuring cylinder to dilute
the sample and obtaining a total solution weight in the
range 5 to 10 g. The solution weight was recorded. 4. The
diluted solution was mixed well before measuring its
refractive index (RI).
5. The diluted solution’s composition was obtained from
the calibration curve.
6. The actual sample’s composition was calculated.
Preparation of Calibrating Curve Procedure.
1. A set of mixtures containing ethanol and water
was prepared within a specified range of
composition between pure water and pure ethanol.
2. The refractive index reading was obtained for
each mixture using a refractometer.
3. The calibrating curve of RI versus composition for
the whole range of mixtures was plotted.
4. The calibrating curve was used to determine the
diluted samples solution’s composition of the
distillation process.
Purity of ethanol: %
Density of ethanol: g/mL
Density of water: g/mL

Amount of Amount of Ethanol Composition Refractive Index

Ethanol (mL) Water (mL) Mol Fraction Weight Percent (RI)

0.0 10.0

1.0 9.0

2.0 8.0

3.0 7.0

4.0 6.0

5.0 5.0

6.0 4.0

7.0 3.0

8.0 2.0

8.5 1.5

9.0 2.0

9.5 0.5

10.0 0.0

Table 6.1: Sample table for preparation of calibration curve

 Tray Temperature Sample Weight Solution Weight Refractive Index

(˚C) (g) (g) (RI)

Distillate

10

Bottom

Table 6.2: Temperature taken for each trays and Refractive

Index (RI) readings for the samples taken
 Table 6.3: Compositions of diluted solution and actual sample

Refractive Index (RI) Diluted Solution’s Actual Sample’s Actual Sample

Composition (wt%) Composition (wt%) Composition (mol%)