CLB20804 – MASS TRANSFER 1 EXPERIMENT 1

1.0 SUMMARY:

A packed column distillation process experiment was conducted with the goal of
understanding the operation of vapor – liquid separation, analyzing the sample for the
top and bottom product by refractometer to obtain the refractive index (RI) in order to
determine their respective composition and also to obtain the time when the vapor –
liquid separation is nearly finish. In this experiment 30 liters of 10% v/v
(volume/volume) mixture of Ethanol in water was prepared and filled in a reboiler
vessel. The mixture was allowed to boiled until almost all component with low boiling
point has been vaporized from the mixture. Temperature readings of all Temperature
Indicator, samples from the Reboiler and the overhead from the Sampling Port were
observed and recorded for every 5 minutes. The concentration of the samples drawn
was measured using refractometer. After analyzing the data collected from this
experiment, it was found that the refractive index obtained for top product is 1.361 and
for bottom product is 1.333 thus, the top product was Ethanol while the bottom product
was water. The time obtained for the vapor – liquid separation is nearly finish was 30
minute because the temperature reading was almost constant at 20-30 minutes after
boiled. This led to a conclusion that this method used for the separation of Ethanol-
water mixture can be considered a reasonably reliable method.

2.0 OBJECTIVE:
 To operate vapor – liquid separation process using a Packed Column
Distillation Unit.
 To analyze the effect of reflux ratio on separation of ethanol-water
system.
 To determine the number of stages by using McCabe Thiele method

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3.0 INTRODUCTION & THEORY:

Distillation is one of the important unit operations in many chemical industries and has
been used from the inception of chemical and process industry. The aim of this experiment was
to carry out batch distillation on a binary mixture using a packed column distillation and
determine the number of stages obtained in the graph that has been construct based on the result.
Distillation is a process where liquid or vapor mixture of 2 or more substance is separated by
the application of removal heat based on their physical properties, specifically, relative’s
volatilities. . A liquid can be classified as volatile when it is readily vaporized at a relatively
low temperature. . The boiling of the more volatile components of the mixture drives the
distillation process. When the vapor is cooled, the more volatile material condenses in a greater
proportion than the less volatile material. The Distillation Column is usually a vertical column
where the liquid and vapor phases of the mixture are made to mix and approach equilibrium.

There are several type of distillation column and each designed to perform specific
types of separation and each differs in term of complexity.For the type of column which is batch
distillation column, it is simple distillation, also known as Rayleigh distillation or differential
distillation, is the most elementary example of batch distillation. In this distillation system, the
vapor is removed from the still during a particular time interval and is condensed in the
condenser. Next, continuous column, there no interruption occurs unless there is a problem with
the column or surrounding process unit. They are capable of handling high throughputs and are
the most common of the two types, trays column, and packed column.

The feed tray divided into a top section and the bottom section. The feed flows down
the column where it is collected at the bottom in the reboiler. The liquid mixture that is to be
processed is known as the feed and this is introduced usually somewhere near the middle of the
column to a tray known as the feed tray.

The reboiler has been obtained the heat to generate vapor. The source of heat input can
be any suitable fluid, although in most chemical plants this is normally stream. In vapor raised
in the reboiler is re-introduced into the unit at the bottom of the column. The liquid removed
from the reboiler is known as the bottom product.

The liquid mixture that is to be processed is known as the feed and this is introduced
usually somewhere near the middle of the column to a tray known as the feed tray. The vapor
moves up the column, and as it exits the top of the unit, it is cooled by a condenser. Holding
vessel known as reflux drum used to store the liquid that has been condensed. Then some of
this liquid will be recycled back to the top column and this known as reflux but when the

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condensed liquid removed from the system called as distillate or top product. If 100% of liquid
recycled back to the column so there no top product. And the reflux ratio will be 1. In addition,
there are internal flows of vapor and liquid within the column as well as external flows of feeds
and product streams and out of the column.

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4.0 RESULTS AND DATA

Table below shows the refractive index and the mole fraction of ethanol.

Table 1: Calibration Table for Ethanol – Water Mixtures

Mole Fraction of
Percent Ethanol % Ethanol (ml) Water (ml) RI
Ethanol
0% 0 20 1.3301 0.0000
5% 1 19 1.3303 0.0160
10% 2 18 1.3303 0.0331
15% 3 17 1.34025 0.0516
20% 4 16 1.34072 0.0716
25% 5 15 1.34059 0.0933
30% 6 14 1.3511 0.1168
35% 7 13 1.3513 0.1425
40% 8 12 1.3514 0.1706
45% 9 11 1.3514 0.2016
50% 10 10 1.3515 0.2358
55% 11 9 1.3515 0.2738
60% 12 8 1.35165 0.3164
65% 13 7 1.3516 0.3643
70% 14 6 1.3516 0.4186
75% 15 5 1.3517 0.4807
80% 16 4 1.3517 0.5524
85% 17 3 1.3517 0.6361
90% 18 2 1.3517 0.7352
95% 19 1 1.3518 0.8543
100% 20 0 1.3518 1.000

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From data obtained from the table 1, a graph of equilibrium curve was plotted as
figure 1 below.

RI vs Mole Fraction Equilibrium Curve

1.36
y = 0.0168x + 1.3415
1.355
R² = 0.3744
1.35
Refractive Index

1.345

1.34

1.335

1.33

1.325
0 0.2 0.4 0.6 0.8 1
Mole Fraction

Figure 1: Graph of refractive Index versus mole fraction of ethanol

The graph above shows the refractive index versus mole fraction of ethanol. This
graph was used to calculate the mole fraction of the top product and bottom product
based on the equation y = 0.0168x + 1.3415.

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Reflux Ratio 1.0

Table 2.1: Data for Reflux Ratio 1.0

Top Product Bottom Product

Time (min)
RI Mole fraction RI Mole Fraction

0 1.340 0.2358 1.336 0.0358

5 1.343 0.095 1.335 0.0355

10 1.343 0.095 1.338 0.0363

15 1.342 0.092 1.335 0.0355

20 1.347 0.1102 1.335 0.0335

25 1.35 0.1150 1.336 0.0358

30 1.351 0.1165 1.334 0.0350

Reflux Ratio 2.0

Table 2.2: Data for Reflux Ratio 2.0

Top Product Bottom Product

Time (min)
RI Mole fraction RI Mole Fraction

0 1.357 0.1187 1.333 0

5 1.353 0.1176 1.333 0

10 1.351 0.1168 1.333 0

15 1.351 0.1168 1.333 0

20 1.348 0.1155 1.33 0

25 1.348 0.1155 1.33 0

30 1.346 0.1148 1.33 0

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5.0 DISCUSSION:
Packed columns are used for distillation, liquid-liquid extraction and gas absorption.
The gas-liquid contact in a packed column is continuous as in a plate column. The vapour or
gas moves up the column and the liquid flows counter-currently down in the column over a
packing surface. The performance of a packed column is very dependent on the maintenance
of good liquid and gas distribution through the packed bed.

Reflux is used by large scale industrial fractionation towers to achieve more efficient
separation of products. Reflux refers to the portion of the condensed overheated liquid
product from a distillation tower that is returned to the upper part of the tower. The down
flowing reflux liquid provides cooling and partial condensation of the up flowing vapors
inside the tower, thus increasing the efficacy of the distillation tower. When the reflux
increase, the better the tower’s separation of the lower boiling from the higher boiling
components of the feed. A balance of heating with a reboiler at the bottom of a column and
cooling by condensed reflux at the top of the column maintains a temperature gradient (or
gradual temperature difference) along the height of the column to provide good conditions for
fractionating the feed mixture.

For this experiment in part A, 21 test tube labelled from A1 to A21 with increasing
concentration of ethanol from test tube A1 until test tube A21. For each test tube, refractive
index was obtain from refractometer and shows an increasing data from 0% of ethanol which
is 1.3301 to 100% of ethanol which is 1.3518. From data obtained, a graph of equilibrium
curve was plotted.

RI vs Mole Fraction Equilibrium Curve

1.36
y = 0.0168x + 1.3415
1.355
R² = 0.3744
1.35
Refractive Index

1.345

1.34

1.335

1.33

1.325
0 0.2 0.4 0.6 0.8 1
Mole Fraction

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The graph above shows the refractive index versus mole fraction of ethanol. This graph was
used to calculate the mole fraction of the top product and bottom product based on the
equation y = 0.0168x + 1.3415. From the graph, the higher the mole fraction of ethanol, the
higher the refractive index is.

For part B, the total mixture of ethanol and water consist of 3 litre of ethanol and 27
litre of water is poured. Based on the boiling point, ethanol has lower boiling point compare
to water which means ethanol is more volatility than water. So, ethanol will be the top
product as it will evaporate, reaching its boiling point first and water will be the bottom
product. The refractive index for pure water and pure ethanol was taken before the
experiment is carried out in part A which is 1.3301 and 1.3518 respectively. In order to fulfil
the objective to analyze the effect of reflux ratio on separation of ethanol-water system two
different reflux ratio is used which are 1.0 and 2.0

The sample from the top product which is ethanol and from the bottom product which
is water is collected for every 5 minutes in 30 minutes for both reflux ratio. The refractive
index for each sample is obtain by using refractometer while the mole fraction is obtained
from the calibration curve. First is the data for reflux ratio 1.0. For top product, at 0min,
5min, 10 min, 15 min, 20 min, 25 min and 30 min, the refractive index is 1.340, 1.343, 1.343,
1.342, 1.347, 1.350 and 1.351 respectively and the mole fraction is 0.2358, 0.0950, 0.0950,
0.0920, 0.1102, 0.1150 and 0.1165 respectively. For the bottom product, at 0min, 5min, 10
min, 15 min, 20 min, 25 min and 30 min, the refractive index is 1.336, 1.335, 1.338, 1.335,
1.335, 1.336 and 1.334 respectively and the mole fraction is 0.0358, 0.0355, 0.0363, 0.0355,
0.0355, 0.0358 and 0.0350.

Next is the data for reflux ratio 2.0. For top product, at 0min, 5min, 10 min, 15 min,
20 min, 25 min and 30 min, the refractive index is 1.357, 1.353, 1.351, 1.351, 1.348, 1.348
and 1.346 respectively and the mole fraction is 0.1187, 0.1176, 0.1168, 0. 1168, 0.1155,
0.1155 and 0.1148 respectively. For the bottom product, at 0min, 5min, 10 min, 15 min, 20
min, 25 min and 30 min, the refractive index is 1.333, 1.333, 1.333, 1.333, 1.330, 1.330 and
1.330 respectively and the mole fraction are all 0.

A complete overall and component mass balance calculation is done based on the
results obtained. There are 2 way to calculate stage, 1st is by graphical method and 2nd is by
analytical method but analytical method only valid for total reflux ratio. Based on the
experiment, 2 Mc-Cabe Thiele graph is plotted which are for reflux ratio 1.0 and for reflux

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ratio 2.0. for the reflux ratio of 1.0, the number of stages is 5 while for reflux ratio of 2.0, the
number of stages is 3. This show that reflux ratio 1.0 is the best reflux ratio because it has
more stages than reflux ratio 2.0. The more the stages occurs in the McCabe Thiele Method
graph the more pure the products of distillation produce or the mixture is highly separated.

There are some errors occurs while conducting the experiment. First is the condition
of the refractometer is not in good condition. It gives inaccurate reading of refractive index.
Next, the reflux ratio is not constant throughout the experiment as the experimenter carelessly
did not stay all the time to maintain the reflux ratio throughout the experiment.

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6.0 CONCLUSION:

In this experiment, all the objectives were achieved which we know how to operate
vapour-liquid separation experiment using a packed column distillation process unit. We also
can do the analysis of the top and bottom samples by using Refractometer to obtain the
Refractive Index in order to we determined their respective composition. From the experiment,
obviously vapor-liquid separation principle can be applied to separate the mixture of ethanol-
water by using packed column distillation process unit. Theory state that the boiling point for
ethanol is (78 ) and water is (100 ). The separation is based on the boiling points of the
mixture components. This make ethanol was the light product due to lower boiling point and
water is heavy product. By using McCabe Thiele Method, the purity of main product was 100%
vaporized at the distillate. However, the number of stages was different due to the reflux ratio.
Two different reflux ratios were tested to determine the Refractive index. Based on the data
collects show that the reflux follows the theory which the theory said that number of stages
will decreases as the reflux ration increases. For reflux 1.0 it has four stages and reflux 2.0 has
two stages.

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7.0 RECOMMENDATION:

There are some improvement that can be made in this experiment to obtained more precise
result. Firstly, Before the experiment is conducting, make sure that we check all the material
and apparatus that we want to use. In this experiment used of Refractometer is also vital. Slight
mistake from calibration will resulting in poor results and at the same time will only make the
plotting of graph more complicated. Next, when testing the sample using Refractometer make
sure ethanol does not vaporize because this can affect the data collected. For another error
which is temperature, the temperature should be set below than the boiling point of ethanol. So
ethanol can be separate than water according to their boiling point. Furthermore, the technician
has to do some maintenance on all the apparatus in the lab. For example, the packed column
flowrate cannot be adjusted because it is constant at 8L/min. We all know that the price of the
packed column is very expensive thus the best way to reduce operating costs of existing units,
is to improve their efficiency and operation via process optimisation and control. To achieve
this improvement, a thorough understanding of distillation principles and how distillation
systems are designed is essential. Lastly, the experiment can be successful if the reboiler is
turned off after reach the maximum temperature which is not higher than boiling point of
ethanol. It can prevent ethanol mixed and vaporized easily with water.

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8.0 REFERENCE:

1. Perry, Robert H. Don Green. Perry’s Chemical Engineering Handbook, Sixth Edition,
McGraw Hill International Edition, New York, 1993.

2. FG, Lab Manual Mass Transfer Packed Column Distillation Process, Universiti Kuala
Lumpur MICET, Melaka,2017

3. Louis Theodore and Francesco Ricchi. (2010). Mass Transfer Operation for the
Practicing Engineer. Canada: John Wiley & Sons, Inc

4. Chilton, T. H., & Colburn, A. P. (1935). Distillation and absorption in packed

columns A convenient design and correlation method. Industrial & Engineering
Chemistry, 27(3), 255-260.

5. Noeres, C., Kenig, E. Y., & Gorak, A. (2003). Modelling of reactive separation
processes: reactive absorption and reactive distillation. Chemical Engineering and
Processing: Process Intensification, 42(3), 157-178.

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9.0 APPENDIX

Part A: calculation of mole fraction

Ethanol 5%

Density of ethanol = 0.789 g/mL

Molecular Weight of Ethanol = 46.07 g/mol

Volume of ethanol = 1 ml

0.789𝑔/𝑚𝑙 × 1𝑚𝑙
Mol of solute = = 0.017126 mol
46.07 𝑔/𝑚𝑜𝑙

Water 95%

Density of Water: 1 g/mL

Molecular Weight of Water: 18.0153 g/mol

Volume of water = 19 ml

1 g/mL x 19 mL
Mol of water = = 1.0546 mol
18.0153 g/mol

Mole Fraction = mole of ethanol / total mole

0.017126 mol
= = 0.016 mol
1.07172 mol

Part B: Convert Feed to Flowrate

789 g/L x 3 L
3L Ethanol = = 51.38 mol
46.07 g/mol

1000 g/L x 27 L
27L Water = = 1498.73 mol
18.0153 g/mol

51.38 mol
Molarity Ethanol = = 1.903 mol/L
27 L

Flowrate = 1.903 mol/L x 30 L = 57.09 mol

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Ethanol Mole Percent:

51.38 mol
Ethanol = x 100% = 3.3 %
1550.11 mol

Water Mole Percent:

1498.73 mol
Water = x 100% = 96.7 %
1550.11 mol

Reflux Ratio 1.0

XD = 0.5524

57.09 Mol

3.3 % Ethanol

96.7 % Water

XF = 0.033 B

XB = 0.0160
F=D+B

57.09 Mol = D + B

D = 57.09 – B

F (XF) = D (XD) + B (XB)

57.09 (0.033) = 0.5524 D + 0.0160 B

1.88397 = 0.357 (57.09-B)+ 0.0160B

1.883397 = 31.5365 – 0.5524B + 0.0160B

B = 52.5724mol

D = 57.09 – 52.5724

= 4.5146 mol
Reflux Ratio : 2.0
Theoretical stages = 5-1 = 4
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Reflux Ratio 2.0

XD = 0.2738
F

57.09 Mol

3.3 % Ethanol

96.7 % Water

XF = 0.033 B

XB = 0.0160

F=D+B

57.09 Mol = D + B

D = 57.09 – B

F (XF) = D (XD) + B (XB)

57.09 (0.033) = 0.2738 D + 0.0160 B

1.88397 = 0.2738(57.09 – B) + 0.0160B

1.88397= 15.6312 – 0.2738B + 0.0160B

B = 53.3252 mol

B = 57.09 – 53.3252

= 3.7648 mol

Theoretical stages = 3-1 = 2

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TOP PRODUCT BOTTOM PRODUCT

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FEED DISTILLATION PACKED COLUMN

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