UNIVERSITY OF TECHNOLOGY, JAMAICA

Faculty of Engineering & Computing

Laboratory Report

Title of Experiment: Continuous distillation column

Experiment #: 4 A-C
Date: February 23, 2016
INSTRUCTOR: Mr Sahlu Baker

COURSE NAME: Unit Operations Laboratory 2

PROGRAMME: Chemical Engineering
SUBMITTED BY: Adrian Fagan, Ronaldo Dixon, Jason Smith
DATE SUBMITTED: March 8, 2016
ID Nos Respectively: 1301500, 1301284, 1104822

Title: Continuous distillation column

Experiments Aim:
A. To determine the pressure drop over the distillation column for various boil-up rates
B. To use the refractometer to determine the composition of the mixture
C. To determine the overall column efficiency at various boil-up rate
Background:
The process of distillation involves the conversion of a liquid to a vapor which is
subsequent condensed to a liquid phase. Its basic operation requires the utilization of a still or
retort (reboiler) which holds the liquid or liquid mixture which is to be vaporized, a condenser to
cool the vapor and a receiver to collect the distillate. In the still (boiler) the mixture is subjected
to heat and the most volatile or the lowest boiling distills first and the others follow based on
their boiling points or not at all. This operation serves as a means of purifying a liquid containing
nonvolatile material. Also, it is highly efficient in separating liquids of widely divergent boiling
points. For laboratory uses, the apparatus is usually made of glass and connected with corks,
rubber bung or ground-glass joints. (Macabe,1993)
Distillation columns are designed with components which are in fixed locations,
components such as downcomers, trays and weirs. Due to the fact that they are in fixed locations
they will tend to have some impacts on the operation of the distillation column, these said
components present a form restriction or resistance to the flow of the vapor and liquid
throughout the column. It is also noted that the flow of the liquid phase is usually very small
when compared to the flow of the vapor phase, with this being said the resistance which is
measured in pressure drop would therefore be significant when the vapor flowrate is increased
beyond its design value. The total pressure across each tray is the sum of that caused by the

resistance of the columns design components and that caused by the passing through of the
liquid on top the tray. The flow of the liquid and the vapor is controlled by varying the boil-up
rate which is done by varying the power input to the reboiler.
Samples from the column may be taken from the bottoms and products outlet and tested
for composition using the refractive index. The refractory index or the index of refraction is a
measure of the bending of a ray of light when passing from one medium into another.
Additionally, refractive indices vary with composition as well as wavelengths of light, and are
frequently noted along with their respective wavelengths therefore, the refractive index therefore
may be used to determine the composition of a substance. In determining the number of
theoretical plates for a given separation at total reflux the following formula known as the
Fenske formula is applicable:

Where n is the number of theoretical plates, Xa is mole fraction of more volatile component, Xb is
the mole fraction of the least volatile component and aav is the average relative volatility (which
is the product of the relative volatility of the combined substances). The Fenske equation was
derived on the assumption that the relative volatility is constant in the distillation column.
The number of theoretical plates obtained by using the Fenske equation can be further
used to determine the column efficiency of the column. The column efficiency in regards to a

distillation column is also referred to as the ratio of the number of theoretical plates and actual
number of plates and is established as the following formula:

E=

Number of theoretical plates

Number of actual plates

* 100

Since an actual, physical plate is rarely a 100% efficient equilibrium stage, the number of actual
plates is more than the required theoretical plates.

Na =

NT
E

Where, Na is the actual physical plates or trays, NT is the number of theoretical plates or trays and
E is the plate or tray efficiency. It is known that a number of factors have an influence on the
column efficiency. These are inclusive of: the type of carrier gas and its flowrate, the compound
and its retention and the column dimensions. Column efficiency has a high dependency the
number of plates, a column with high plate numbers are known to have higher column efficiency
than columns with a lower plate numbers. A high column efficiency is often an indication of a
narrower peak at a given retention time than a column of lower efficiency. High column
efficiency also includes less peak separation to completely resolve narrow peaks.

Methodology:
As outline in the lab manual with the following change:

Methylcyclohehane replaced with ethanol.

Toluene replaced with tap water.

Apparatus:
Figure 1. Showing apparatus used in this experimental exercise

Part A
Results;

Table 1 Showing reesults obtained when the power inputs were varied

Power
(kW)

Boil-up Rates
(L/hr)

Pressure Drop
(cms H2O)

Degree of Foaming
Tray 1

0.5

Tray 5

1.034

62

Gentle localised

None

1.651

65

Gentle localised

Gentle localised

2.712

68

Violent localised

Gentle localised

3.750

70

Gentle over entire tray

Violent localised

4.615

72

Violent over emtire tray

Gentle over entire

tray

Violent over emtire tray

Violent over
emtire tray

0.75

1.00

1.25

1.50

1.75
5.450

Treatment of results

74

Table 2 Showing Varying Power Inputs and Their Relevant Log Pressure Drops and Log
Boil Up Rates

Power Inputs (kW)

Log Pressure Drop

Log Boil Up Rates

0.5
0.75
1.00
1.25
1.50
1.75

1.792
1.813
1.83
1.845
1.857
1.869

0.015
0.218
0.433
0.574
0.664
0.736

Figure.2 Showing the plot of Log Pressure Drop VS Log Boil Up Rates

Log-Log graph showing pressure drop vs boil up rate

1.88
1.86
1.84
1.82
Log Pressure Drop

1.8
1.78
1.76
1.74
0

0.1

0.2

0.3

0.4

0.5

Log Boil Up Rates

Part B

0.6

0.7

0.8

Table 4. Showing results the refractive index obtained at the different %composition

Composition
(%)

REFRACTIVE INDEX

SAMPLE 1

SAMPLE 2

SAMPLE 3

AVERAGE

100

19.4

19.3

19.3

19.3

75

20.2

20.0

20.0

20.1

50

19.6

19.7

19.5

19.6

25

16.5

16.2

16.3

16.3

Treatment of results:

Figure 3. Showing a plot of refractive index versus percentage composition of the

water/methanol mixture

Refractive index vs mole fraction of ethanol

25

20

15

Refractive index
10

0
0

0.2

0.4

0.6

0.8

mole fraction of ethanol

Part C

1.2

The following Table displays the mole fraction of Ethanol and Water present in the distillate and
bottom for each trial. These data point were all obtained by entering the column temperature and
refractive index of ethanol sample into the Engineering Equation Solver. The program calculated
the mole fraction of ethanol present in each sample, from which the mole fraction of water could
be calculated.

Table 6. Showing Results Obtained for Partial Pressure at the Different

Column Temperatures

Mole Fraction
Power

Species

Distillate

Bottom

0.5

Ethanol

0.968

0.068

0.974

0.104

0.980

0.129

0.992

0.189

0.977

0.197

0.981

0.142

Water
0.75

Ethanol
Water

Ethanol
Water

1.25

Ethanol
Water

1.5

Ethanol
Water

1.75

Ethanol
Water

Table 7.Showing results obtained after completing a series of calculations

using the partial pressure values obtained from table.6

Power (KW)
Efficiency (E)%
0.5
69.2
0.75
66.9
1.0
67.1
1.25
71.6
1.5
61.0
1.75
66.5
Average Efficiency (E)%
67.05

Sample calculations
For the first trial, (Power of 0.5 kW):
To determine alpha, equation 11.17 from the Coulson and Richardsons Chemical Engineering
Volume 2 text will be used. This equation will be used under the assumption that the system
under investigation is ideal.
Therefore:
o

P
= 0A
PB
The Engineering Equation Solver software was utilised to determine the vapour pressure of
ethanol and water at the average column temperature. These values were then substituted into the
equation above.
Hence, in the first trial:
d=

PA
PB

 b=

PA
PB

b b
av =

Now using Fenskes Equation:

log
n+1=

X A XB
x
XB X A
log AB

n=

The efficiency is given by;

E=

of theoritical plate
x 100=
of actual plate

Hence first trial:

Power (0.5kW):

d=

166.7 x 10 3
44.08 x 103
d
3

b=

172.7 x 10
3
45.86 x 10
b=3.766

= 3.782

3.782 3.766
av=
av =3.774

Now using Fenskes Equation:

log
n+1=

log AB

log
n+1=

X A XB
x
XB X A

Methanol

P A = 166.7

172.7

Water

PB = 44.08

45.86

0.968
10.068
x
10.968
0.068
log 3.774

n+1=

2.617
0.577

n+1=4.536

n= 5.536
The efficiency is given by;

E=

of theoritical plate
x 100=
of actual plate

E=

5.536
x 100=69.2
8

Adrian Fagan (1301500)

Discussion
Throughout the experiment, generally, it was seen that as the input power increased, the pressure
drop of the vapour also increased. This increase in pressure drop also varied directly with the boil
up rate. This is due to the fact that the internals of the distillation column is fixed hence all these
internals represent a frictional or resistance force that acts against the liquid and vapor flows
taking place inside the column. The liquid flows are normally very small in comparison to the
vapor flows and thus the resistance confronted by the vapor (measured in pressure drop) is very
significant when the vapor flow rate is increased beyond its design value. Since the liquid feed to
the column can be consider constant therefore when the heat input increases to the reboiler, this
increases the vapor flow up the column against the same liquid flow that the column was
designed for. Therefore, the vapor flow generates more pressure drop due to more resistance

resulting from excess vapor trying to ascend through a fixed path. In layman terms, it can be
consider cramming more vapor through a resistance that was designed for less vapor flow.
Ideally, the graphical relationship between the pressure drop and the boil up rate should be an
exponential one in which the two variables are directly proportional. That is, as the pressure drop
increases, the boil up rate also increases. However, this trend was not completely followed in
actuality. Although, there was a general increasing trend there were some fluctuations throughout
the experiment. These fluctuations in the boil up rate can be attributed to human errors such as
reaction time. The refractive index simple describes how light propagates through the mixture.
From the graph a general correlation can me use to determine the composition of ethanol based
on the refractive index

The boiling point of the mixture can be higher than the boiling point of the less volatile
compound, or lower than the boiling point of the more volatile compound at some molar
compositions. When this happens the resulting mixture is called an azeotrope. When this
happened, it means that the mixture of the two compounds cannot be further separated into pure
compounds through distillation. Our two compounds, water and ethanol, form such an azeotrope,
with the boiling point of the mixture dropping below the boiling point of pure ethanol, the more
volatile of our two compounds. This can be seen on the vapor-liquid equilibrium curve, where
the molar fraction of the ethanol in the liquid in our curve is higher than the molar fraction of
ethanol in the vapor. Part c of this experiment deals with the the overall column efficiency at
various boil-up rate With an increase in the power input to the reboiler, there was an increase in
composition of the distillate and the bottom. These values obtained were not always consistent

therefore it could be safe to say that the fluctuations in the power and temperature at various
instances in the experiments may affect the readings.

Conclusion
Based on the results, the pressure drop of the distillation column was determined to have
a proportional relationship to the boil up rate. Refractive index can be used to determine the
composition of a mixture. The column efficiency calculated using partial pressure values and
Fenske s equation was found to be 67.05%.

Jason Smith 1104822

Discussion:
This laboratory experiment consisted of three (3) different experiments. The first was
done with the aim to determine the pressure drop over the distillation column for various boil-up
rates. The boil-up rate was manipulated by increasing the power input to the reboiler for each
trial by 0.25 kW for a range of 0.5 1.75 kW. The pressure was measured in cm H2O using a
manometer. From the data collected, it can be seen that the pressure drop increased steadily and
proportionally relative to the boil-rate. This is correlated by the graph of Log Pressure drop vs.
Log Boil-up rate that was plotted. The degree of foaming in the Trays 1 and 5 of the distillation
column exhibited bubbling and splashing of liquid based on the power level. Both trays
progressively transitioned from gentle localized to violent over entire tray with Tray 5 show
no sign of foaming initially. In a distillation column the liquid flows downwards while the

vapour flows upwards. The liquid flows under the influence of gravity through the trays while
the vapour travels upwards due a pressure gradient being present. This means if there is no
pressure drop between the trays, the vapour will not flow. That would mean that there would be
nothing to collect in the condenser. With a greater pressure drop with an increase in the boil-up
rate, it would indicate that a greater vapour flow occurs with an increase in the power input to the
reboiler.
The second experiment was carried out with the aim to use the refractometer to determine
mixture composition. A refractometer is an instrument used to measure the speed of light. The
reading on the device related to the speed of light in air. This comparison is called refractive
index. This property is a value specific to a material and depends on temperature and wavelength
(colour) of the light. Using a refractometer, you will be able to determine the concentration of a
material, if temperature and wavelength are known. Varying composition of water-ethanol
mixture was analysed , ranging from 100% ethanol to 0% in 25% increments. Three (3) samples
were done for each trial and the average calculated. The refractive index for ethanol was
basically constant except when the property was determined for a composition of 25%. This can
be seen from the graph that was plotted of Refractive Index vs Mole Fraction of Ethanol.
Although the refractive index was relatively constant, it did not progress proportionally with
regard to the composition. This could be due to an error in the creation of the water-ethanol
mixture. The error from the device would already be accounted for by taking three (3) data sets
for each composition.
The third experiment was conducted with the aim to determine the overall column
efficiency at varying boil-up rates. With an increase in the power input to the reboiler, there was
an increase in composition of the distillate and the bottoms to a point. At that point there was a

drop in the values observed. This can be attributed to the fact that water and ethanol is an
azeotropic mixture. This means that their mixture can either have a higher boiling point than
either of the components or they can have a lower boiling point
There were fluctuations in the power and temperature at various instances in the
experiments. Also the flow rate of the condensate had to be kept constant to maintain equilibrium
conditions. These factors could have contributed errors to the data collected for the experiments
done.

Conclusion:
In conclusion the pressure drop over the distillation was related proportionally to the boilup rates with the degree of foaming increasing proportionally to the level of power input to the
reboiler. The pressure drop varied from 62 cm H2O at 0.5 kW of power input to 74 cm H2O at
1.75 kW of power input. The refractive index of a mixture of 25% composition ethanol was 16.3
compared to 19.3 for a composition of 100% ethanol. The column efficiency calculated using
partial pressure values and Fenske s equation was found to be 67.05%.

Discussion: Ronaldo Dixon 1301284

In this experiment the mixture placed in reboiler was an ethanol-water mixture, the most
volatile component of the two being ethanol with a boiling point of 78.4 C. By convention, the
liquid that vaporizes first would be ethanol as its vapor pressure comes into equilibrium with the
surrounding pressure at a lower temperature. The main objective of this experiment was to
determine the pressure drop across the column for varying boil-up rates. The boil-up rate was
controlled by the power input connected to the reboiler. Through observation it was seen that as
power increased so too did the pressure drop across the column, an observation which holds true
to convention therefore validating the operations of the experiment. From a theoretical stand
point it can be explained that as the power is increased the degree of volatilization is increased
and by convention the vapor would have a higher flowrate than that of the liquid therefore the

flow of vapor would increase and this increase in velocity would result in an increase in pressure
drop.
From the log-log graph showing pressure drop versus boil-up rate it was also evident
that boil-up rate is proportional to pressure drop, as the pressure drop increases likewise would
there be an increase in boil-up rate. In reference to the refractive index it can be said that the
mole fraction of ethanol should some form of proportionality to the refractive index, as mole
fraction increased likewise did the refractive index until at about a range of 0.2-0.5 where it
became debatably constant.
Conclusion:
After thorough observations and calculations it may be concluded that the boil-up rate is directly
proportional to the power input and the pressure drop across the column. In addition, the pressure
drop may also be affected by the degree of foaming in the tray, from observation it was validated
that increases in power input resulted in an increase in the degree of foaming.

REFERENCES
Seader, J. and Henley, E. Separation Process Principles. John Wiley & Sons, 1998, Chapters 7
and 8.

McCabe, Warren. Unit Operations of Chemical Engineering, Fifth Edition. McGraw-Hill, Inc,
1993, Chapters 18 and 19.
Distillation Column Design. Copyright 1997