EPF 3105 Food Process Engineering

Laboratory 2

Tittle: Experiment 4- Distillation

LECTURER NAME : Dr. Roseliza Binti Kadir Basha
SESSION TIME : Wednesday (2.00P.M. - 5.00PM)
GROUP : 4

GROUP MEMBERS:
Lee ZiQing 168587
Nur Leha Binti Mansor 170016
Norhafiza Binti Kamal 170078
NurAin Binti Mohd Jaafar 167219
Siti Nur Adibah Binti Hamzah 167259


Faculty of Engineering

UN I V E R S I T I PU T R A MA L A Y S I A
Title: Experiment 4: Continuous Distillation Column
Introduction:
Distillation is the oldest method used for separating mixtures of liquids.
Distillation exploits the fact that different liquids have different boiling points. When a mixture
of liquids is heated, the liquid with the lower (or lowest) boiling point vaporizes first. That vapor
is routed through a condenser, which cools the vapor and causes it to condense as a liquid; the
liquid is then collected in a receiving vessel. As the original liquid mixture continues being
heated, eventually, some or all of the lower-boiling liquid is driven off, leaving only the higher-
boiling liquid or liquids in the distillation vessel.
Distillation is an imperfect method for separating mixtures of liquids that form azeotropes.
An azeotrope, also called a constant boiling mixture, is a mixture of two or more liquids at a
specific ratio, whose composition cannot be altered by simple distillation. Every azeotrope has a
characteristic boiling point, which may be lower (a positive azeotrope or minimum-boiling
mixture) or higher (a negative azeotrope or maximum-boiling mixture) than the boiling points of
the individual liquids that make up the azeotrope.
Ethanol forms a positive azeotrope with water. The boiling point of a mixture of 95.6%
ethanol (by weight) with 4.4% water is 78.1 C, which is lower than the boiling point of pure
water (100 C) or pure ethanol (78.4 C). Because the azeotropic mixture boils at a lower
temperature, its impossible to use simple distillation to produce ethanol at concentrations higher
than 95.6%. (More concentrated ethanol solutions can be produced by using drying agents such
as anhydrous calcium chloride that physically absorb the water from a 95.6% solution of ethanol.
These solutions must be stored and handled carefully, because otherwise they absorb water vapor
from the air until they reach the 95.6% azeotropic concentration.)
Ethanol also forms azeotropes with many other liquids, including some that are
poisonous or taste bad. This allows production of denatured ethanol, which is toxic, cannot be
drunk and so can be sold cheaply without cannibalizing sales of (and taxes on) much more
expensive potable ethanol, such as vodka and other distilled beverages.

Objective:
1. To separate two component of a miscible liquid-liquid mixture by using a distillation
column.
Materials and apparatus:
1. Ethanol
2. Water
3. Distilled water
4. Conical flask
5. Beaker
6. Refractometer
7. Distillation column
Procedure:
1. A volume of ethanol was mixed with a volume of water and the refractive index of the
initial mixture was recorded.
2. The mixture in the reboiler section of the distillation column was boiled.
3. Sample from product stream (V3) on every 5 minutes was collected and the refractive
index was recorded.
4. Concentration of the product from stream (V3) was obtained from standard curve.
5. Sample from bottom stream (V2) were collected on every 5 minutes and the refractive
index were recorded.
6. Concentration of the product from stream (V2) was obtained from standard curve.
7. Graph of refractive index versus concentration was plotted.




Result:
Time taken for the distillation process to complete=45 minutes
Refractive index of mixture (initial) = 9.9
Refractive index of product collected (ethanol) = 4.8
Refractive index of mixture in reboiler at the end of the experiment= 7.4
Table 1: Reading for Standard Curve
Concentration of Ethanol (%) Refractive Index (RI)
10 3.2
20 6.3
30 9.5
40 12.2


Graph 1: Standard Curve of Refractive Index of Ethanol in Various Concentrations

0
2
4
6
8
10
12
14
0 10 20 30 40
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Concentration of Ethanol (%)
Standard Curve
Table 2: Sample from product stream (V3)
Concentration of ethanol (%) Refractive Index
0.055 1.7
0.112 3.5
0.130 4.1
0.135 4.2
0.135 4.2
0.140 4.3
0.140 4.3
0.142 4.4
0.150 4.7
0.155 4.8



Graph 2: Curve for Sample from Product Stream (V3)

0
1
2
3
4
5
6
0.055 0.112 0.13 0.135 0.135 0.14 0.14 0.142 0.15 0.155
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Concentration of Ethanol (%)
Cuve for Product Stream (V3)
Table 3: Sample from product stream (V2)
Concentration of ethanol (%) Refractive Index
0.350 10.1
0.318 9.9
0.318 9.9
0.310 9.7
0.295 9.2
0.285 8.8
0.278 8.7
0.250 7.8
0.245 7.7
0.238 7.4


Graph 3: Curve for Sample from Product Stream (V2)


0
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4
6
8
10
12
0.35 0.318 0.318 0.31 0.295 0.285 0.278 0.25 0.245 0.238
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Concentration of Ethanol (%)
Curve for Product Stream (V2)
Discussion:
Modern distillation is multi-stage, continuous, counter-current, vapor-liquid contacting
systems that operate in different materials that boil at different temperature. Throughout this
experiment, we have deeply understood the process of distillation. We studied the process going
on distillation column. In the experiment, we truly understand how ethanol was separated from
water. Water and ethanol were heated in the reboiler. Water has higher boiling point than ethanol
which is 100C and 78.9C respectively. When the mixture had reached the temperature of
78.9C, ethanol was first boiled and evaporates as vapor. The vapor was then arrived at the
condenser; cooled water at the condenser condensed the vapor resulting from the boiling process.
After condensation, it was spitted into two streams. One stream is for pure ethanol and another
stream is the reflux which is return to the top of tower to supply the liquid downflow required in
the upper portion of the tower.
Based on the procedures stated in lab manual, we are supposed to calculate the
concentration of V2 and V3 by measuring the density of solution. Due to the pycnometer cannot
be used during the experiment; we had come to another way to calculate the concentration of V2
and V3. We were asked to plot a standard curve of refractive index versus the concentration of
ethanol (%). Thus, we prepared various concentration of ethanol in water. We had 10%, 20%, 30%
and 40% of ethanol concentration in water, and then we measured the refractive index by using
refractometer. A straight standard line was plotted to obtain the concentration of V2 and V3 in
experiment.
In the experiments, we took V2 and V3 on every 5 minutes after mixture in reboiler had
boiled. This purpose is to determine the change of concentration and refractive index of V2 and
V3 on every 5 minutes. The measurement of refractive index has a wide variety of applications.
It is commonly used to identify a particular substance, determine its purity, or measure
concentration. Refractive index is nearly linearly related to the percentage of ethanol in a
solution. By comparing the value of the refractive index of a solution to that of a standard curve
the concentration of solute can be determined with good accuracy.
Based on the graph, we can see the curve for product stream (V3) increase. We can say
the concentration of ethanol increase when the higher refractive index of ethanol. Whereas we
can see the curve for bottom stream (V2) is decreasing. This is because the ethanol in reboiler
had been decreasing, thus the RI decrease when the concentration decrease. Therefore we can
conclude that, the relationship between RI and Concentration of ethanol is related. We can say
the RI increase, when the concentrations of ethanol increase.
Refractive index is a number that describe how light propagates through that medium.
The refractive index determines how much light refracted when entering a material. Refractive
index once described by Snells law of refraction is the angle of incidence and refraction. This is
why the refractive index is high when concentrations of solution increase. The high
concentration solution caused the refracted angle to be high. Thus, refractive index is high.
Conclusion:
As a conclusion, the mixture of ethanol and water must reach the ethanols boiling point
so that the process can be carried out. When the mixture had reached its boiling point, which is
78.9C, thus the distillation process (the separation of ethanol and water) will be started. Ethanol
is denser compared to water, so that it will conclude why the product stream (V3) produce
ethanol and the other stream which is bottom stream (V2) produce water.
Since the pycnometer are not available during the experiment, the concentration of the
mixture are determined by using the standard curve that have been prepared based on the various
concentration of ethanol which are 10%, 20%, 30% and 40 %. Then, the concentration of ethanol
and water for every 5 minutes can be determined by using the concentration standard curve as
the benchmark.
The graph of product stream (V3) is increasing. The reading of refractive index for
ethanol keeps increasing as the time increase prove that the ethanol are becoming more
concentrate for every 5 minutes. While the refractive index of water decreasing as the time
increasing proving that the concentrations of ethanol are increasing. Thus thats why the graph
for bottom product (V2) is decreasing. This is because the refractive index was measured to
identify the concentration of the liquid. So, as the time increasing, the concentrations of ethanol
are increasing and make both of the streams produce high concentration of ethanol.
Based on the experiment, we can conclude that the refractive index will increase as the
concentration increased. Both of the liquids were successfully separated by using the distillation
column and the graph has proved that the refractive indexes are dependent on the concentration.
Reference:
1. Castillo, M., Roerig, A.T., Walsh, M. (2006). Relationship Between Index of Refraction
and Concentration of Trihexylmethylammonium. Retrieved from
http://www.usd.edu/arts-and-sciences/chemistry/northern-plains-undergraduate-research-
center/upload/StdntGrp_Pres_Isnt_it_Ionic.pdf
2. Tham, M.T. (2009). Distillation an introduction. Retrieved from
http://lorien.ncl.ac.uk/ming/distil/distil0.htm
3. Freuhauf, P.S., & Mahoney, D.P. (2014). Distillation Column Control Design Using
Steady State Models: Usefulness and Limitations. Retrieved from
http://www.aspentech.com/publication_files/Distillation_Column_Control_Design_Using
_Steady_State.pdf
Appendix:

Figure 1: Distillation Column

Figure 2: Distillation Chamber

Figure 3: Refractometer

Figure 4: Samples of ethanol and ethanol water mixture