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0 SUMMARY
The main objectives of this experiment are to operate vapor liquid separation
process using a Bubble Cap Column Distillation Unit, and also to analyze the sample for the
top and bottom product by refractometer to obtain the refractive index. Other objective is to
calculate the number of stages by using McCabe Thiele method. In distillation process, the
purities of distillate are depending on some factors such as the operating time, temperature,
reflux factor and chemical properties. 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. On this experiment the component
that use is ethanol and water with the ratio of 3:27 which is 3 liters of ethanol and 27 liters of
water. At the bottoms contain mixture of ethanol and water heated around 70C and 90C
where is in the range of ethanol boiling point. The top product is contains of mostly pure
ethanol which is obtained from the condensation process. The purities of distillate
composition are determined by reflection index measurement. The data taken in every 5
minutes and recorded.For the first set of reflux ratio which is at 1.0, the top product gives the
value of 1.360 of refractive index. While at bottom product the refractive index is 1.332.
While the second experiment is 2.0 reflux ratio, the result shows that the top product
refractive index is 1.356 and for the bottom product refractive index is 1.331. It can be say
that, the distillation process already separate the ethanol and reach its initial purity. The reflux
ratio is important because it give influence on the number of tray required.
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2.0 OBJECTIVES
To operate vapor liquid separation process using a Bubble Cap Distillation 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 calculate the number of stages by using McCabe Thiele method.
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3.0 INTRODUCTION AND THEORY
of purity nor temperature through conversion of a liquid into vapor that is subsequently
condensed back into liquid. Distillation is widely used for separating mixtures or product in
industries.
alcoholic liquors from fermented materials, or in the separation of two or more liquids having
different boiling points, as in the separation of gasoline, kerosene, and lubricating oil from
crude oil. Other industrial applications include the processing of such chemical products as
formaldehyde and phenol and the desalination of seawater. The distillation process appears to
have been utilized by the earliest experimentalists. Aristotle (384322 bc) mentioned that
pure water is made by the evaporation of seawater. Pliny the Elder (ad 2379) described a
primitive method of condensation in which the oil obtained by heating rosin is collected on
different substances readiness to become a vapor. If the difference in boiling points between
distillation. If the boiling points differ only slightly, many re distillations may be required. If
a water and alcohol distillate is returned from the condenser and made to drip down through a
long column onto a series of plates, and if the vapor, as it rises to the condenser, is made to
bubble through this liquid at each plate, the vapor and liquid will interact so that some of the
water in the vapor condenses and some of the alcohol in the liquid vaporizes.
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The feed tray divides the column into a top (enriching or rectification) section and a
bottom (stripping) section. The feed flows down the column where it is collected at the
bottom in the re boiler. Heat is supplied to the re boiler to generate vapor. The source of heat
input can be any suitable fluid, although in most chemical plants this is normally steam. In
refineries, the heating source may be the output streams of other columns. The vapor raised in
the re boiler is re-introduced into the unit at the bottom of the column. The liquid removed
from the re boiler is known as the bottoms product or simply, the bottoms. The vapor travels
up the column, and as it exits the top of the unit, it is cooled by a condenser. The condensed
liquid is stored in a holding vessel known as the reflux drum. Some of this liquid is recycled
back to the top of the column and this is called the reflux. The condensed liquid that is
Most methods of distillation used by industry and in laboratory research are variations
of simple distillation. But still there are a few method of distillation such as fractional
distillation, vacuum distillation and Azeotropic distillation. Each method of distillation have
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their own benefits to the process. But each distillation column will used different type of
packing. Examples of common packing that were used in industries are packed column and
bubble cap. There were other type of pack or tray such as pro-pak,heli-
Bubble-cap tray is device or packing that was mounted in a rectifying column that
concentrates the alcohol. Vapor from the still pot rises into the column and enters a pipe on
the bottom of the tray. The cap forces the vapor into the liquid sitting on top of the tray.
Some of the vapor condenses overflows the weir on the tray and falls down the column.
Some of the alcohol in the liquid vaporizes creating a higher concentration of alcohol and
rises further in the column where the process is repeated at the net bubble cap tray. The caps
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4.0 DATA AND RESULT
A1 0 20 1.331 0
A2 1 19 1.333 0.015955475
A3 2 18 1.334 0.033097026
A4 3 17 1.336 0.051562012
A5 4 16 1.339 0.071509854
A6 5 15 1.342 0.093126648
A7 6 14 1.344 0.116630989
A8 7 13 1.346 0.142281191
A9 8 12 1.348 0.170385834
A21 20 0 1.360 1
Table 1: Data recorded to obtain references graph of mixture of ethanol and water
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4.2 GRAPH FOR REFERENCE
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4.3 CALCULATION FOR FEED LINE MOLAR FRACTION XF
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4.4 DATA AND RESULT FOR BUBBLE CAP DISTILLATION WITH
REFLUX RATIO: 1.0
Rotameter reading R1 (L/hr) = ________ 3______
Table 2: Data obtain from bubble cap distillation of mixture ethanol and water by using the
value of reflux ratio: 1.0
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4.4.1 MATERIAL BALANCE (REFLUX RATIO: 1.0)
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GRAPH 2 : MOLE FRACTION OF ETHANOL IN VAPOR (Y) VS MOLE FRACTION OF
ETHANOL IN LIQUID (X) FOR REFLUX RATIO: 1.0
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4.5 REFLUX RATIO= 2.0
Rotameter reading R1 (L/hr) = _________1.4_________
Table 3: Data obtain from packed column distillation of mixture ethanol and water by using
the value of reflux ratio: 2.0
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4.5.1 MATERIAL BALANCE (REFLUX RATIO: 2.0)
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GRAPH 3 : MOLE FRACTION OF ETHANOL IN VAPOR (Y) VS MOLE FRACTION OF ETHANOL IN
LIQUID (X) FOR REFLUX RATIO: 2.0
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5.0 DISCUSSION & ANALYSIS
In this experiment, we were operating bubble cap distillation equipment. The purpose
each stage consist of a tray designed to contact raising vapor with descending liquid, which
increases the vapor composition of the more volatile component. Data of the top and bottom
product which is the refractive index value were collected and analyzed, the efficiency of
There were three graph obtained. First, there is a reference graph where the data were
collected from a sample of series of measured ethanol and water mixture. It was used to
obtain the molar fraction of mixture of ethanol and water distillate in bubble cap distillation.
Moreover, there were two different reflux ratio value being experimented. Reflux
ratio is the ratio of reflux flow to distillate flow and is a measure of how much of the material
going up the top of the column is returned back to the column as reflux. As we compare the
results obtained, it shows that the refractive index of reflux ratio 1.0 is increasing with time
while for reflux ratio 2.0 the refractive index is decreasing as time increases. Based on the
observation, we found that the more liquid that is rich in the more volatile components are
From graph 2 and 3, McCabe Thiele method was applied in order to determine the
number of stages. Based on graph 2, which is for reflux ratio 1.0, the value of X D is 1.00, XF
is 0.26, and XB is 0.02. By constructing the graph with the value obtained, the number of
stages cannot be identify and therefore we could not get to know how much the plates
available. However, for graph 3, number stages is 1 and no plates require. The value for XD
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There are very high different in the value of distillate when comparing the result in
graph 2 and graph 3. The experiment by using reflux ratio more higher give out a lover mole
fraction of ethanol in liquid phase. Normally, less reflux ratio, the more stages needed to
reach the desired composition plus if the reflux ratio decreases, then its arriving at a condition
where rectifying, stripping and the feed line intersect at the equilibrium line. However, the
results are differ from the theory, the main error caused by the reflux ratio setting. During the
process, the reflux ratio is not constantly stable and it need to be monitored well.
Distillation process is consist of binary mixture that needed to be purified by the help
of stages and plates. The error of this experiment especially on the first one may due to the
fact that the concentration of the binary mixture was taken as an approximation. The
temperature kept fluctuating from time to time and therefore we could not get a steady state
of temperature when taking stage readings for both top and bottom products.
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6.0 CONCLUSION & RECOMMENDATION
In conclusion, from distillation by using reflux ratio with value of 2 gets no plates but
only consist of 1 stage. However distillation by using reflux ratio equal to 1:1 does not give
any clear reading of stages because we get total 100% of ethanol in distillate top product.
Vapour-liquid separation through distillation was studied using bubble cap distillation
process unit. In trays and bubble cap distillation tower the holes in each tray are covered with
caps called bubble caps. The slots in these bubble caps disperse the raising vapor through the
liquid on the tray. Each bubble cap has many slots and each tray has many bubble caps to
spread up the vapor. This ensures maximum contact between vapor and liquid and ensures
the maximum of mass transfer between liquid and vapour. Based on the data obtained, the
refractive index for top and bottom product was analysed thus, the top product was Ethanol
while the bottom product was water. The time obtained for the vapour liquid separation is
nearly finish was 30 minute. It can be concluded that this method used for the separation of
Ethanol-water mixture can be considered a reasonably reliable method. This experiment can
be improved by taking the data more than once. Other than that, the condition of machine
order to achieve more accurate result. Besides that, lab manual also should be read properly
before entering the laboratory to avoid any misunderstanding, misconception in order to run
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7.0 REFERENCES
1) http://www.che.ufl.edu/unit-ops-lab/experiments/Distillation/CD-Operating-
Instructions.pdf
3) Azyyati Binti Johari, Mass Transfer Chapter 2 Power Point Slide Note, UNIKL
MICET, 2014, Page 95
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8.0 APPENDIX
Test Tube Volume of Ethanol Volume of Water(m3) Mass of Mass of Mol of Mol of
(m3) Ethanol(kg) Water(kg) Ethanol(mol) Water(mol)
A0 0 0.000020 0 0.02 0 1.11111111
A1 0.000001 0.000019 0.000789 0.019 0.017114967 1.0555555556
A2 0.000002 0.000018 0.001578 0.018 0.034229935 1
A3 0.000003 0.000017 0.002367 0.017 0.051344902 0.9444444444
A4 0.000004 0.000016 0.003156 0.016 0.068459872 0.8888888889
A5 0.000005 0.000015 0.003645 0.015 0.085574832 0.8333333333
A6 0.000006 0.000014 0.004734 0.014 0.102689805 0.7777777778
A7 0.000007 0.000013 0.005523 0.013 0.119804772 0.7222222222
A8 0.000008 0.000012 0.006312 0.012 0.136919743 0.6666666667
A9 0.000009 0.000011 0.007101 0.011 0.154034707 0.6111111111
A10 0.000010 0.000010 0.007890 0.01 0.171149675 0.5555555555
A11 0.000011 0.000009 0.008679 0.009 0.188264642 0.5
A12 0.000012 0.000008 0.009468 0.008 0.205379513 0.4444444444
A13 0.000013 0.000007 0.010257 0.007 0.222464577 0.3888888889
A14 0.000014 0.000006 0.011046 0.006 0.239609544 0.3333333333
A15 0.000015 0.000005 0.011835 0.005 0.256724512 0.2777777778
A16 0.000016 0.000004 0.012624 0.004 0.273839479 0.2222222222
A17 0.000017 0.000003 0.013413 0.003 0.290954447 0.1666666667
A18 0.000018 0.000002 0.014202 0.002 0.308069414 0.1111111111
A19 0.000019 0.000001 0.014992 0.001 0.325184382 0.0555555556
A20 0.000020 0 0.015780 0 0.342299349 0
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TEST TUBE TOTAL MOLE OF ETHANOL MOLE FRACTION OF REFRACTIVE INDEX
AND WATER ETHANOL
A0 1.111111111 0 1.331
A1 1.072670523 0.015955475 1.333
A2 1.034229935 0.033097026 1.334
A3 0.995729347 0.051562012 1.336
A4 0.957348759 0.071509854 1.339
A5 0.918908171 0.093126648 1.342
A6 0.880467583 0.116630989 1.344
A7 0.842025994 0.142281191 1.346
A8 0.803586406 0.170385834 1.348
A9 0.765345818 0.201314185 1.350
A10 0.726705234 0.235514577 1.353
A11 0.688264642 0.273535252 1.357
A12 0.640824054 0.316054182 1.355
A13 0.611383466 0.363919846 1.356
A14 0.572942878 0.418208435 1.358
A15 0.534502291 0.480305729 1.357
A16 0.496061702 0.552027053 1.358
A17 0.457621114 0.635797691 1.358
A18 0.419180525 0.734932554 1.357
A19 0.380139937 0.854085295 1.358
A20 0.342299349 1 1.360
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8.2DATA FOR EQUILIBRIUM LINE
0.00 0.00
0.05 0.38
0.10 0.53
0.40 0.75
0.60 0.79
0.80 0.86
0.94 0.94
0.90 0.91
0.94 0.94
0.96 0.96
0.98 0.99
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