OBJECTIVES

 To be able to operate a Vapour-Liquid Separation Experiment using a Bubble Cap

Distillation Process Unit.
 To analyze the sample for the Top and Bottom Product by Refractometer to obtain the
Refractive Index in order to determine their respective composition.
 To obtain the time when the Vapour-Liquid Separation is nearly finish.

SUMMARY

This experiment explained on the distillation process through the usage of the Bubble
Cap Distillation Unit (Shown in Appendices-Figure 1). The purposes of this experiment are
basically to operate a Vapour-Liquid Separation Experiment using a Bubble Cap Distillation Process
Unit, to analyze the sample for the Top and Bottom Product by Refractometer to obtain the Refractive
Index in order to determine their respective composition and to obtain the time when the Vapour-
Liquid Separation is nearly finished. At the end of the experiment, the Refractive Index (RI) for both
Ethanol and Distilled Water were obtained and the average readings were calculated and written down
which are 1.359 and 1.335 respectively. Moreover, a hypothesis was made which is, as the Time
(min) increases, the Refractive Index (RI) for both Ethanol and Distilled water stabilizes uniformly.
As closure, we have learned the distillation process even deeper by studying and understanding the
processes it underwent in order to obtain the desired product, as well as in determining Ethanol and
Distilled Water’s respective composition.
 INTRODUCTION

The experiment of the Bubble Cap Distillation process is about the separation of the
mixture by using bubble cap trays (Appendices-Figure 1). In this case, the operation of the
process is to separate the mixture of vapor–liquid separation. In vapor–liquid separation, the
process can be defined as a process in which a liquid or vapor mixture of two or more
substances is separated into its component fractions of desired purity, by the application and
removal of heat. To remove or separate the mixture to vapor and liquid, the bubble cap tray is
the right instrument in this experiment. The type of column used in this experiment is the
batch column which means a specific quantity of a liquid mixture is separated into its
components.

The experiment will first begin by preparing the mixture into specific quantities. The
composition of the mixture will be tested by using the Refractometer. Then, fill the mixture
or feed into the Reboiler below the maximum level indicated. All valves will be check
whether it is at open or close condition based on the experiment. The cooling water will be
supplied to fill into the Condenser when the experiment begins. The vapor from the mixture
will flow through the distillation unit where the bubble cap trays are placed. It is the place
where the separation of the mixture happens. The product from the distillation unit will flow
through to another unit which is called as the Condenser that acts as a cooling system. The
result from the Condenser will be in liquid state, which appears as a vapor before it was
condensed. The desired product from this experiment is the vapor, but in the end of this
experiment the desired product will change into the liquid state where it will be easily
collected.
 THEORY

This experiment is more about the vapor–liquid separation process. Distillation

(Appendices-Figure 2) for this experiment is based on the fact that the vapor of a boiling
mixture will be richer in the components that have lower boiling points. Therefore, when this
vapor is cooled and condensed, the condensate will contain more volatile components. At the
same time, the original mixture will contain more of the less volatile material. Distillation
columns are designed to achieve this separation efficiently. Because of that, this experiment
has used a vapor–liquid separator.
A vapor–liquid separator is a device used in several industrial applications to separate
a vapor–liquid mixture. For the common variety, gravity is utilized in a vertical vessel to
cause the liquid to settle to the bottom of the vessel, where it is withdrawn. In low gravity
environments such as a space station, a common liquid separator will not function because
gravity is not usable as a separation mechanism. In this case, centrifugal force needs to be
utilized in a spinning centrifugal separator to drive liquid towards the outer edge of the
chamber for removal. Gaseous components migrate towards the center. The gas outlet itself
may be surrounding by a spinning mesh screen or grating, so that any liquid that does
approach the outlet strikes the grating, is accelerated, and thrown away from the outlet.

The best column internals for the instrument used for vapor–liquid separation is the
bubble cap tray. The bubble cap tray has a riser or chimney fitted over each hole to cover the
riser. The cap is mounted so that there is a space between riser and cap to allow the passage
of vapor. Vapor rises through the chimney and is directed downward by the cap, finally
discharging through slots in the cap, and finally bubbling through the liquid on the tray.
 In this experiment, the composition of the mixture will be tested by using the
Refractometer (Appendices-Figure 3). A Refractometer measures the extent to which light is
bent (i.e. refracted) when it moves from air into a sample and is typically used to determine
the index of refraction (aka refractive index or n) of a liquid sample.

The refractive index is commonly determined as part of the characterization of liquid

samples, in much the same way that melting points are routinely obtained to characterize
solid compounds. It is also commonly used to:

 Help identify or confirm the identity of a sample by comparing its refractive index to
known values.
 Assess the purity of a sample by comparing its refractive index to the value for the pure
substance.
 Determine the concentration of a solute in a solution by comparing the solution's
refractive index to a standard curve.

The reflux ratio can assume any number between a minimum value and an infinite
value, and the number of theoretical stages required for separation changes accordingly. The
importance of the reflux ratio is that it can affect the separation efficiency, i.e. xD (mole
fraction of MVC in distillate). The minimum reflux ratio and the infinite reflux ratio place a
constraint on the range of separation operation. The choice of reflux ratio to use is governed
by cost considerations.
 RESULTS

Initial Refractive Index (RI):

Ethanol : 1.359
Water : 1.333

Time Temperature Readings (°C) RI Top RI Bottom

(Min) TI 1 TI 1A TI 1B TI 2 TI 2A TI 2B TI 4 TI 5 TI 6 Product Product
0 32 32 40 31 32 32 44 39 33
5 32 33 40 31 32 31 58 39 32
10 32 33 40 31 32 31 68 39 32
15 32 33 40 31 32 31 62 39 32
20 32 33 40 31 31 30 68 39 32
25 32 33 40 31 32 31 77 39 32
30 32 33 40 31 32 31 83 39 32
35 32 33 40 31 32 31 89 39 31 NO ETHANOL WAS
40 60 78 89 82 88 90 90 39 32 RECOVERED
45 57 81 90 83 89 91 91 39 32 1.358 1.335
50 78 81 90 82 88 91 91 39 32 1.359 1.3355
55 78 80 90 81 87 90 92 39 32 1.359 1.335
60 79 80 90 81 87 91 92 39 32 1.36 1.3355
65 79 80 90 81 87 90 82 39 32 1.36 1.335
70 79 80 90 81 87 91 92 39 32 1.36 1.335
75 79 80 90 81 87 81 93 39 32 1.36 1.335

Table 1: Table of Raw Data

 PROCEDURES

Starting up, 27 L of distilled water and 3 L of ethanol were prepared in their

respective containers (pail). Both solutions were then mixed until the solutions turn
homogeneous, and this will be summed to a total sample volume of 30 L. Then, the prepared
sample (water + ethanol mixture) was poured into the Reboiler at the Separation Unit. Next,
the Reboiler was switched ON to allow the sample to be heated. Also, the voltage value was
set to 230 V. While the sample is being heated by the Reboiler, the readings of the
thermocouples (TI 1, TI 1A TI 1B, TI 2, TI 2A, TI 2B, TI 4, TI 5, TI 6) shown at the panel
were recorded, for every 5 minutes, for a total of an hour and 15 minutes. Once the ethanol
(BP=78C) has been condensed, close V2 and open V3. This will able the ethanol condensate
to flow to the Collector at the Separation Unit. Once the ethanol has been collected, the
Refractive Index (RI) of both water and ethanol can be determined with the aid of the
Refractometer. To shut down the process, the power switch of the Reboiler was switched off.
Then, the main power control switch was turned off. Next, allow the liquid in the Reboiler to
cool down before draining it out of the system, followed by housekeeping.
 DISCUSSION

This experiment was all about the Bubble Cap Distillation Process. The experiment was also
about to operate a Vapour-Liquid Separation Experiment using a Bubble Cap Distillation Process
Unit, to analyze the sample for the Top and Bottom Product by Refractometer to obtain the Refractive
Index in order to determine their respective composition and to obtain the time when the Vapour-
Liquid Separation is nearly finished. The variables involved in this experiment are Time (Min),
Temperature Readings, TI 1, TI 1A, TI 1B, TI 2, TI 2A, TI 2B, TI 4, TI 5, TI 6 (°C), Initial Refractive
Index (RI) – Ethanol and Water, Refractive Index (RI) of Top Product, and the Refractive Index (RI)
of Bottom Product.

In general, the Bubble Cap Distillation Process Unit comprises of a Reboiler, a Column, a
Condenser, and a Collector which flows accordingly. A specified amount of 27 L of Distilled Water
and 3 L of Ethanol were prepared. Then, both solutions were then mixed until the solution becomes
homogenous which results in a new, 30 L sample. Next, the prepared sample (Distilled Water and
Ethanol mixture) were poured into the Reboiler. The main switch of the Reboiler was then switched
ON and the voltage value was set to 230 V (5 coils) to allow the sample to be heated to a certain
temperature for future experimentations. Furthermore, while the sample is being heated by the
Reboiler, the readings of all the 9 thermocouples (TI 1, TI 1A, TI 1B, TI 2, TI 2A, TI 2B, TI 4, TI 5,
TI 6) were accurately recorded which were shown on the panel for every 5 minutes, for a total of an
hour and 15 minutes. Once the Ethanol (Boiling Point of 78 °C) has been condensed, valve V2 were
closed and valve V3 were opened. These actions will lead the Ethanol to the Collector. Once the
Ethanol is collected, the Refractive Index (RI) of both Distilled Water and Ethanol can finally be
determined.

As for the results, in comparison with the Initial Refractive Index (RI) of both Distilled Water
and Ethanol which are 1.359 and 1.333 respectively, the average Refractive Index (RI) of the Top
Product – Ethanol calculated is 1.359. As for the average Refractive Index (RI) of the Bottom Product
– Distilled Water calculated is 1.335. The average Refractive Index (RI) of the Ethanol and Distilled
Water were both calculated in between the range of 45 min to 75 min. This is because the Ethanol
needs to be at its boiling point (78 C) in order for it to evaporate and flow itself to the Collector in
order to be tested for its Refractive Index (RI) value.
 Theoretically speaking, a vapor–liquid separator is a device used in several industrial
applications to separate a vapor–liquid mixture. For the common variety, gravity is utilized in
a vertical vessel to cause the liquid to settle to the bottom of the vessel, where it is withdrawn.
In low gravity environments such as a space station, a common liquid separator will not
function because gravity is not usable as a separation mechanism. In this case, centrifugal
force needs to be utilized in a spinning centrifugal separator to drive liquid towards the outer
edge of the chamber for removal. Gaseous components migrate towards the center. The gas
outlet itself may be surrounding by a spinning mesh screen or grating, so that any liquid that
does approach the outlet strikes the grating, is accelerated, and thrown away from the outlet.

There are several possibilities that might have contributed to the errors that occurred
during the experiment. One of those errors is physical errors (human error). The parameters
weren’t allowed to be stabilized first when the readings were recorded, which could lead to
an abnormal trend of results. Not just that, the parameter in the field of another parameter
might have been recorded due to lack of focus. By doing so, the recordings will be inaccurate
and it will result in abnormality in the trend of results. Thus, the ideal expected results could
not be achieved. Besides that, the wires or other equipment involved may be faulty or not
plugged in. When this happens, the panel will not display the correct value and could even
disrupt the whole process of the experiment. Not just that, the temperature of the system may
be set too high (above 100 C). In the event of this fault, the water could evaporate together
with the ethanol, and this will end with an impure product (ethanol + water instead of pure
ethanol).
 CONCLUSION

In conclusion the flow and process of the Bubble Cap Distillation process were
explained in this experiment. The data and information were collected and recorded and were
utilized in operating a Vapour-Liquid Separation Experiment using a Bubble Cap Distillation Process
Unit, in analysing the sample for the Top and Bottom Product by Refractometer to obtain the
Refractive Index in order to determine their respective composition and in obtaining the time when
the Vapour-Liquid Separation is nearly finished. After all the data were written down, the average
Refractive Index (RI) of both Ethanol and Distilled Water can finally be calculated which are 1.359
and 1.335 respectively. In comparison with the Initial Refractive Index (RI) of both Ethanol and
Distilled Water which are 1.359 and 1.333, it can be observed that there was not much difference in
its reading. In addition to that, a hypothesis was made which is, as the Time (min) increases, the
Refractive Index (RI) for both Ethanol and Distilled water stabilizes uniformly. From that, the
objectives were achieved.

RECOMMENDATIONS

To prevent physical errors (caused by experiments) from occurring, focus and

patience play a huge role to record any data. Also, work together to record data, and not just
be dependent on just a team member. Next, in order to prevent recording the wrong data,
team members should reconfirm with each other on the results to acquire the readings which
best fit. Early precautions are important so that the experiment can be carried out smoothly
without any unwanted errors. Make sure to read the lab manual before going through with the
experiment to get a brief idea on how to conduct the experiment. This step is really important
so that the experimenters know what to do in the lab rather than waiting for the technicians to
guide them through until the end and to prevent any amateur hour. Furthermore, prioritizing
the instrument’s condition is really important as it will affect the results. Asking the
technician to check on the instrument beforehand is strongly recommended. Ensure that the
temperature (< 80 C), as well as the voltage value is configured correctly to attain smooth
run of the experiment and in order to obtain the ideal product. This will prevent the water to
evaporate alongside the ethanol.
 REFERENCES

[1] M.T. Tham (1997-2009). Distillation, [Online]. Available from:

http://lorien.ncl.ac.uk/ming/distil/distil0.htm [25th March 2014]
[2] Anonymous A (2014). Vapor-Liquid Separator, [Online]. Available from:
http://en.wikipedia.org/wiki/Vapor%E2%80%93liquid_separator [25th March 2014]
[3] Hanson J. (2003). Refractometry, [Online]. Available from:
http://www2.ups.edu/faculty/hanson/labtechniques/refractometry/intro.htm [25th March
2014]
APPENDICES

Figure 1-Bubble Cap Trays

Figure 2-Distillation Process

Figure 3-Refractometer