Technological Institute of the Philippines - Manila
(CHEP 510L1, 2nd Semester, SY 2015-2016)
DISTILLATION
Princess Consulta, Ma. Heresa Diamante, John Dolph Facundo,
Mark Carlo Guevarra, April Joy Haro
ABSTRACT
The unit operation distillation is a method used to separate
the components of a liquid solution, which depends upon the
distribution of these various components between a vapor and a
liquid phase. All components are present in both phases. The
vapor phase is created from the liquid phase by vaporization at
the boiling point.
Distillation is concerned with solutions where all
components are appreciably volatile, such as in ammonia-water
or ethanol-water solutions, where both components will be in
vapor phase.
The percent ethanol extracted will be calculated with the use
of pycnometers. Each pycnometer was weighed first and then
filled with water. Then, it is measured using OHaus analytical
balance (Model No. PA214) to calculate for the mass of water
inside the pycnometer.
Distillate of the distilling column and placed inside the
pycnometer. Then, we measured again its mass using also
OHaus analytical balance (Model No. PA214).
After the experiment was conducted, the percent ethanol in
the distillate will be calculated using the density and values
acquired using pycnometer.
I. INTRODUCTION
The unit operation distillation is a method used to separate the
components of a liquid solution, which depends upon the
distribution of these various components between a vapor and a
liquid phase. All components are present in both phases. The vapor
phase is created from the liquid phase by vaporization at the boiling
point.
The basic requirement for the separation of the components by
distillation is that the composition of the vapor be different from the
composition of the liquid with which it is in equilibrium at the
boiling point of the liquid. Distillation is concerned with solutions
where all components are appreciably volatile, such as in ammonia-
water or ethanol-water solutions, where both components will be in
vapor phase. In evaporation, however, of a solution of salt and water,
the water is vaporized but the salt is not. The process of absorption
differs from distillation in that one of the components in absorption
is essentially insoluble in the liquid phase. An example is absorption
of ammonia from air by water, where air is insoluble in the water-
air ammonia solution.
Batch Distillation
In a batch distillation, it is invariably the overhead product or a
cut of it that is required and there are generally two methods of
operation by which the top product or products are obtained.
1. Varying Reflux. This is used to obtain an overhead product of
constant composition. As the top product composition becomes
richer in heavier components due to the removal of the lighter
fractions, the reflux ratio is increased to maintain a constant
composition. This is continued until there is so little top product
that the still is virtually running at total reflux and the operation
becomes uneconomic to proceed further.
2. Constant Reflux. Under these conditions the overhead product
.
1
composition continually changes, gradually becoming richer in
the less volatile components. One or more cuts can be taken at
various intervals to give top products of required composition.
This experiment demonstrates the use of constant reflux to
obtain a top product of a specified average composition (0.95
mole fraction of ethanol) by batch distillation of a binary
mixture of ethanol and water of composition 60% w/w.
Reflux Ratio
In large scale and industrial operations, the reflux ratio
plays an important part, both economically and practically in
the design and operation of such units. The reflux ratio can be
defined as the weight of the top product removed as product. At
total reflux, infinite reflux ratio, the separation achieved is
maximum. However this is the least economic method of
operation because the amount of product is minimum and large
supply of energy are required in heating the mantle.
At the other end of the scale, working at zero reflux, all top
products are removed, the separation achieved is a minimum.
In this case, to achieve a desired top product a column of
maximum height is required.
Therefore, a balance has to be found to minimize the cost of
the column, in terms of height, diamter, running costs,
compatible with a specified top product, by using the optimum
reflux ratio to achieve this.
This experiment demonstrates the variations in top product,
which can be achieved, in a column of fixed dimensions, solely
through variation of the reflux ratio.
Vacuum Distillation
The relative ease of separation of a binary mixture can be
readily determined by inspecting the vapor-liquid
composition/temperature curve (commonly known as lens
diagram due to its shape). Separation will be easy if the lens is
a flat one and more difficult if it is a thin one, providing no
complications occur e.g. presence of azeotropes. This diagram
varies with pressure in several ways.
Decreasing the total pressure on the system lowers the
whole diagram, thus boiling points are obviously reduced under
reduced pressure. Conversely, increasing the total system
pressure decrease the relative volatility of the components with
respect to each other and this shows as a thinning in the lens
diagram making separation more difficult. Due to the increased
pressure, boiling points will also be increased. However, if the
total pressure of the system is increased to the critical pressure
of one of the components, complete separation becomes
possible. It can be seen therefore that operation under vacuum
should lead to a more efficient separation of the feedstock
mixture. In the following experiments, the effects of vacuum on
the binary system of ethanol / water are investigated.
 Distillation

II. MATERIALS & METHODS

The ethanol-water solution used inside the distilling column is

provided by TIP-Manila Chemical Engineering Laboratory.
The following apparatus were used: five 25-ml pycnometer, five
APPENDICES
250-ml beaker, 25-ml pipette, aspirator bulb, and analytical balance.
The equipment used in this experiment is the distilling column Documentation
inside the unit operations laboratory provided by the TIP-Manila
Chemical Engineering Laboratory.
OHaus analytical balance (Model No. PA214) is used by the
researchers to weigh reagents accurately.

III. EXPERIMENTAL SETUP

Each pycnometer was weighed first and then filled with
water. Then, it is measured using OHaus analytical
balance (Model No. PA214) to calculate for the mass of
water inside the pycnometer.
After a while, samples were taken at the bottoms and
distillate of the distilling column and placed inside the
pycnometer. Then, we measured again its mass using also
OHaus analytical balance (Model No. PA214).
The weight of the samples is used to calculate the
volume and density of the mixture.

IV. RESULTS & DISCUSSION

Figure 1. Weighing of Water and Pycnometer

Sample Temperature, Mass of Density , Percentage

C mixture, kg/m3 of Ethanol
g
1 83 24.7852 821.5834 55.1715
2 80 26.5405 829.504 54.3459
3 82 26.9215 841.4099 48.4184
4 82 26.9425 843.0148 47.7257

The preceding table shows the percentage of ethanol in the

distillate. From the original 50:50 solution of ethanol and water we
can see that the percentage of ethanol increases.
This behavior can be attributed by the principles of evaporation
inside the distilling column. Ethanol has a lower boiling point thus
the first one to go into the distillate.
However, at some point there is an accuracy of the values
obtained due to some impurities left in the distilling column from
the past experiments.

V. CONCLUSIONS Figure 2. Sample Distillate

It can be concluded that distillation is of assistance in
separating liquids through differences in boiling points. This
was observed in the increased concentration of ethanol in the
distillate as compared with the concentration of ethanol in the
feed.

However, there is an observed inaccuracy in obtaining

the mass percent of ethanol through density. The densities
obtained were higher than the density of pure water and pure
ethanol. The ethanol present in the column from previous
experiments could be a source of impurity that may have
oxidized to acetaldehyde. Even though there were impurities
present while conducting the experiment, the separation of
two components was observed applying the concept of binary
distillation.

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 Technological Institute of the Philippines - Manila
(CHEP 510L1, 2nd Semester, SY 2015-2016)
From Perrys Handbook:
Density of pure ethanol at 82C= 736.9501612 kg/m3
Density of pure water at 82C = 970.5446 kg/m3

Basis: 100 kg ethanol-water mixture , Let x= kg of ethanol

100/ (x/736.9501612 + 100-x/ 970.5446) = 841.409

x= 48.4184 kg
%ethanol = 48.4184 kg /100kg x 100 = 48.4184 %

Trial 4:

Mass of pynometer= 22.9795

Mass of water = 55.0786g - 22.9795= 31.9957g
Mass of ethanol-water = 498621- 22.9795= 26.9425g
Desity of ethanol-water = 26. 9425g / 31.9957g = 0.8430147968=
843.0147kg9/m3

From Perrys Handbook:

Fig.3 Putting samples inside the pycnometer Density of pure ethanol at 82C= 736.9501612 kg/m3
Density of pure water at 82C = 970.5446 kg/m3
Calculation
Basis: 100 kg ethanol-water mixture , Let x= kg of ethanol
Trial 1:
100/ (x/736.9501612 + 100-x/ 970.5446) =843.0147
Mass of pynometer= 24.911g
x= 47.7257 kg
Mass of water = 55.0786 g - 24.911g = 30.1676g
%ethanol = 47.7257 kg /100kg x 100 = 47.7257 %
Mass of ethanol-water = 49.6962- 24.911g= 24.7852g
Density of ethanol-water = 24.7852g / 30.1676g = 0.8215834206
= 821.5834206 kg/m3
ANOVA Result:
From Perrys Handbook:
Using EZANOVA, the effect of temperature with the % ethanol
Density of pure ethanol at 83C= 730.40272 kg/m3
extracted was tested.
Density of pure water at 83C = 970.0731 kg/m3

Basis: 100 kg ethanol-water mixture , Let x= kg of ethanol

100/ (x/730.40272 + 100-x/ 970.0731) = 821.5834206

x= 55.1715kg
%ethanol = 55.1715 kg /100kg x 100 = 55.1715%

Trial 2:

Mass of pynometer= 22.9795

Mass of water = 54.9752 g - 22.9795= 31.9957g
Mass of ethanol-water = 49.52- 22.9795= 26.5405g
Desity of ethanol-water = 26.5405g / 31.9957g = 0.829502=
829.502kg/m3

From Perrys Handbook:

Density of pure ethanol at 80C= 738.642528 kg/m3
Density of pure water at 80C = 971.8007 kg/m3

Basis: 100 kg ethanol-water mixture , Let x= kg of ethanol

100/ (x/738.642528 + 100-x/ 971.8007) = 829.502kg

x= 54.34589862 kg
%ethanol = 54.34589862 kg /100kg x 100 = 54.34589862 %
With the p value of less than 0.000394 the effect of temperature
with the % ethanol extracted was significant. Therefore, in
Trial 3:
distillation, temperature greatly affects the solubility of the
components and determines the mass of the component you want to
Mass of pynometer= 22.9795
recover.
Mass of water = 55.0786g - 22.9795= 31.9957g
Mass of ethanol-water = 49.901- 22.9795= 26.9215g
Desity of ethanol-water = 26. 9215g / 31.9957g = 0.8414099=
841.409 kg9/m3

3
 Distillation

Acknowledgment

The authors would like to thank the CHEP 510L1 adviser, Engr.
Crizaldy V. Tugade, for his unwavering support and guidance for
the realization and the fulfillment of the intended learning outcomes
of the course. They also extend their candid appreciation to the
Chemical Engineering Laboratory and Chemical Engineering
Department for providing the materials and equipment needed as
well as their educational motivation to pursue for greater and better
learning.

REFERENCES
[1] Geankoplis, C. J. (1995). Transport Processes and Unit
Operations, 3rd Ed. Singapore: Prentice Hall.
[2] Perry, R. H., & Green, D. W. (2008). Perry's Chemical
Engineering Handbook, Eight Edition. New York: McGraw-
Hill.