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Binary Distillation

University of Illinois at Chicago

Binary DistillationPre Lab

This schematic illustrates what happens in a distillation column. A liquid mixture is fed into the
distillation column. On entering the column, the heated feed is partially vaporized and rises up
the column. However, as it rises, it cools by contacting the descending cooler liquid and partially
condenses so that, while part of vapor continues to flow upward, the condensed portion is
enriched in the less volatile component(s) and flows downward. As the vapor continues to flow
upward, it undergoes partial condensation a number of times and each time becomes richer in the
more volatile component(s).
Unit Operations Lab 4
March 11, 2010
Group 3
Shrikant Shah
Brandon Farr
Alex Georg
Michael Ogiefo
Mohammed Khatib
Ghassan Alkhateeb
Unit Operations ChE-382 Group No. 3
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Spring 2010

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Binary Distillation

University of Illinois at Chicago

1.

Table of Contents
WP&C.....................................................................................................................................2

1.

Introduction............................................................................................................................3

2.

Theory......................................................................................................................................5

3.

Apparatus..............................................................................................................................13

4.

Materials and Supplies.........................................................................................................18

5.

Procedure..............................................................................................................................19

8.

Error Analysis.......................................................................................................................21

9.

References.............................................................................................................................22

1. WP&C
What is the purpose of this experiment?
The purpose of this experiment is separate a mixture of a 5% wt methanol-water solution in a binary distillation
column. About 0.1-2 GPM of methanol-water mixture will be introduced into the round bottom flask of the column.
The column will operate at temperatures ranging from 0-100oC. The column will be run and allowed to reach steady
state before samples from the six stages will be obtained and tested with a Refractometer to eventually obtain the
methanol concentration in each stage.
What are the hazards associated with the experiment?
1. Methanol is relatively toxic fluid. It can cause eye, skin and respiratory tract irritation when carelessly
exposed to lab personnel.
2. The electrical wires for the thermocouples are carelessly exposed. If lab personnel were to accidentally touch
them while conducting experiment, they run the risk of an electric shock.
3. The persistent use of fluids like water and methanol could lead to fluid spillage. If lab personnel were to walk
over an affected area, they run the risk of injuries due to a fall.
How will the experiment be conducted in a safe manner?
1. Lab personnel should wear gloves, goggles, slip resistant shoes, and a facemask when conducting experiment
especially when handling the methanol.
2. Paper towels or task wipers should be in close proximity to clean up any fluid spills that may occur during
experiment.
3. The Distillation column should not be heated until the mixture has reached the Reboiler section of unit.

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Spring 2010

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Binary Distillation

University of Illinois at Chicago

What safety controls are in place?


1. There is a failsafe valve present that allows the removal of fluids incase the unit gets flooded.
Describe safe and unsafe ranges of operations.
1. The operating flow rates of water should be between 0-2 GPM. All relevant data can be obtained in this
range. An increase flow rate between 3-10 GPM could be hazardous due to increased pressure.

Signatures:

Shrikant Shah
Brandon Farr
Alex Georg
Michael Ogiefo
Mohammed Khatib
Ghassan Alkhateeb

1. Introduction
Distillation is a physical separation process that uses the differences in volatility between
compounds in a liquid mixture. Binary distillation separates two liquid components from one
another. All fluids possess some degree of volatility that is a measure of their tendency to
vaporize. A higher volatile compound such as methanol will vaporize more quickly when
compared to water under the same atmospheric conditions. Boiling the two components would
also make the difference even more apparent, as the less volatile water would boil at a higher
temperature than the methanol. More importantly, even when two components are mixed
together, the unique physical properties of the individual component still causes the more volatile
component to vaporize faster. This is what ultimately makes distillation possible.
A single step of distillation uses these principles of volatility to achieve a separation of
compounds at equilibrium. At the boiling point of a mixture, the more volatile component exists
as a greater fraction in the vapor than it will in the liquid. In a methanol-water mixture,
distillation would yield a greater mole fraction of methanol in the vapor than in the liquid.
Unit Operations ChE-382 Group No. 3
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Spring 2010

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Binary Distillation

University of Illinois at Chicago

Condensing the vapor and adding more distillation steps or stages in series is the basis for
continuous distillation. When a continuous system is arranged vertically, the system is defined
as a distillation column. In such a column, falling liquids vaporize at lower stages and rising
vapors condense at higher ones. A heat source at the bottom of the column enables this action,
creating a decreasing temperature gradient up the column. With more distillation steps greater
purity can be achieved in top and bottom of the column.
Distillation columns are widely used for separations in industry, most notably in
petroleum, natural gas, and chemical processing, as well as any other large-scale liquid
production. In processing petroleum, different hydrocarbons can be separated according to their
volatility. Medicinal herbs can be distilled from plant matter in the pharmaceutical industry.
Methanol is distilled for high alcohol content products such as whiskey.
In this experiment, we will distill a mixture of methanol and water in a column distiller.
The apparatus has six trays that will act as the stages of the continuous distillation. Collection of
the condensate at each of these stages will allow an analysis of the composition at each plate.
The temperature will also be recorded at each stage. Ultimately, decreasing temperatures and
increasing compositions of methanol will be observed up the column. Finally, vapor-liquid
equilibrium data will allow a comparison between experimental results and theoretical trends.
2. Theory
Distillation is the separation, by vaporization, of different components in a mixture
because of the different volatilities that they possess at a given boiling point of the mixture.
When a mixture reaches a specific temperature and pressure a certain amount of the mixture
moves into the vapor phase until the vapor reaches the mixtures vapor pressure. This point is
known as the vapor-liquid equilibrium. Volatility is a measure of a pure components vapor
Unit Operations ChE-382 Group No. 3
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Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb

Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago

pressure at a set pressure and temperature in a specific mixture. It is incorrectly assumed that the
components of a mixture will separate based on their boiling points when pure. Rather, the
boiling point of a mixture is based on the total vapor pressure of a mixture, which is a sum of the
vapor pressures of each individual component in the mixture. This is known as Daltons law.
sat

P = (v pa + v pb )

(1)

Where,
sat

v pa

[=] Vapor pressure of component a [kPa]

v pb

[=] Vapor pressure of component b [kPa]

[=] Vapor pressure of mixture [kPa]

This means that a component will not boil off cleanly meaning it is impossible through
distillation to obtain a pure substance. The vapor created above a mixture is also a mixture of
components. The composition of the vapor is based on the volatility of each of the substances.
Raoults law helps us to determine what the volatility, or K value of a substance. This in turn
allows us to find the mole fraction of a component in the vapor phase.
y a=

v pa x a

(2)

psat

Where:

ya

v pa

xa

Psat

[=] mole fraction of component a in vapor phase (dimensionless)


[=] vapor pressure of component a [kPa]
[=] mole fraction of component a in liquid phase (dimensionless)
[=] Vapor pressure of mixture [kPa]

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Spring 2010

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Binary Distillation

University of Illinois at Chicago

Not all mixtures obey Raoults law. Some components that have high solubility with each
other form azeotrope. An azeotrope is a mixture that has either a higher or lower boiling point
than the boiling point of any of the pure components. This means that when a mixture reaches an
azeotrope, such as ethanol and water at 95.6 % water, it behaves as a pure substance.
The simplest of all distillation techniques is called flash distillation. Flash distillation occurs
when a mixture at a specific temperature and pressure is allowed to drop in pressure. This
changes the vapor-liquid equilibrium of the mixture and creates a vapor rich in the most volatile
component(s). This is also the crudest form of distillation and does not allow for refinement of
the distillates.
A more complicated form of distillation is batch distillation. Batch distillation uses both a
boiler and a condenser, but only allows one separation, or cut, to be taken from the mixture.

Figure 1: A schematic of a typical continuous distillation tower. A is the kettle that holds the
liquid mixture, B is the Reboiler that adds heat to the mixture, C is the distillation column that
holds the trays or packing, D is the condenser that turns the distillate to a liquid product.

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Spring 2010

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Binary Distillation

University of Illinois at Chicago

Continuous distillation is the most complicated and most common form. It has a boiler,
condenser and multiple trays or packing which allows the vapor to condense as it moves up the
column and cools. The trays or packing allows for a better separation of the components in the
mixture which in the end gives purer products. It also adds a lot of complexity to the system.

Figure 2: A typical tray in a distillation column. A is the tray itself, B are the holes in the tray
that allow the vapor to pass through the tray, C and D are the tubes that allow liquid to pass from
one tray to another. As the vapor moves up the column it gets progressively cooler which allows
some of the mixture to condense and further concentrates the vapor with the lightest
component(s).

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Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago

Figure 3: This shows a simple McCabe-Thiele diagram. The number of steps corresponds to the
number of trays needed for a given mixture.
Determining the size of the tower and the number of trays needed was historically a very
difficult process involving many calculations. The McCabe-Thiele method greatly simplified that
process. The method uses a graphical representation of the material balance equations as
operating lines on a graph of the liquid composition (x-axis) and the vapor composition (y-axis).
The bottom line in Figure 3 is the x-y line. This starts at the origin and ends where x and y both
equal 1.This line would represent a distillation column that operated at total reflux and total boilup, meaning that all of the vapor and all of the liquid is recycled back into the system. The next
line added is the vapor liquid equilibrium line for a binary system which is found
experimentally. By moving step-wise between the two lines we can find the number of
theoretical plates needed for a specific separation of a binary mixture and the liquid and vapor
composition at any point in the distillation column. These stage lines can be seen in Figure 3.

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Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago

Figure 4: McCabe-Thiele diagram with operating lines and feed line added.
In practice, we want to draw a purified product out of the column in the form of either a
distillate (top of the column) or the bottoms product (bottom of the column) or both. This
requires a column that operates at a partial reflux and/or a partial boil-up ratio. This means that
we cannot use the x-y line for such a column. In Figure 4 we see the addition of a line for reflux
ratio (slope L/V) and a line for the boil-up (slope L/V). The boil-up lines slope increases as we
increase the amount of bottoms product that we remove from the system. Subsequently, as we
remove more distillate as product we decrease the slope of the top operating line, which is the
line for the reflux ratio. By changing the amount of liquid re-boiled, which is liquid returned to
the column as a vapor, or by changing the amount of vapor refluxed, returned to the column as a
liquid, we change the number of theoretical plates necessary for a given separation. The q

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Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb

Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago

(quality) line in Figure 4 is the feed line which is the composition of the stream entering the
distillation column. We can see from the diagram in Figure 4 that where that line intersects with
the two operating lines is the feed stage, or the tray at where the incoming stream enters.
The quality q is defined as:
q=

H h f
LL

F
Hh

(3)

Where:

L [=] liquid flow rate below the feed (mol/hr)

[=] quality of the feed (dimensionless)

L [=] liquid flow rate above the feed (kJ/kg)


F [=] feed flow rate (mol/hr)
H [=] saturated vapor enthalpy of feed (kJ/kg)
hf [=] enthalpy of feed (kJ/kg)
h [=] saturated liquid enthalpy of feed (kJ/kg)

The feed line can then be defined as:


y=

ZF

q
( q1
) x + 1q

(4)

Where:

y [=] vapor mole fraction of methanol (dimensionless)


q [=] quality of the feed (dimensionless)
x [= ] liquid mole fraction of methanol (dimensionless)
ZF [=] mole fraction of methanol in feed (dimensionless)

The top operating line is defined as

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Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago


L0
L0
D
D
y=
x + 1
x
L0
L0 D
(1+ )
1+
D
D

( )

(5)

Where:

y [=] vapor mole fraction of methanol (dimensionless)


L0 [=] liquid reflux rate into column (mol/hr)
D [=] distillate flow rate (mol/hr)
x [=] liquid mole fraction of methanol (dimensionless)
xD [=] mole fraction of methanol in distillate (dimensionless)

The McCabe-Thiele method is widely used for binary mixtures. When dealing with multicomponent mixtures addition assumptions and calculations are necessary. There are a number of
issues that need to be watched when sizing a continuous distillation column properly. They are:
Foaming- foaming occurs when the gas passing upward causing the liquid to bubble
excessively. While this normally depends on the properties of the liquid, it can also be caused by
improper tray designs.
Entrainment- Occurs when the vapor velocity is too high due to a column having too
small of a diameter. This causes liquid to be held up at the trays and does not allow proper
circulation of the liquid.
Weeping- Occurs when the vapor velocity is too low. When the velocity drops too low,
liquid starts to fall, or weep, through the holes in the plates. This does not allow enough liquid to
get to the re-boiler which means that the entire column needs to be shut down and re-started.
Flooding- This occurs when liquid entrainment become too severe. This causes a large
pressure drop in the column and contaminates the distillate.

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Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago

3. Apparatus

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Binary Distillation

University of Illinois at Chicago

22
24

T8

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Binary Distillation

University of Illinois at Chicago

Figure 5 represents the Binary Distillation apparatus without any of the support beams. The column is
constructed of a round bottom flask (7) which holds a methanol- water solution. This solution is distilled by
applying electrical energy to the heating jacket (24) which heats up the solution causing the volatile liquids and
gases to rise. Total reflux occurs in the system by feeding cooling water (10) into a cooling coil (16) at the top
of the column. Thermocouples (T1-T9) measure the temperatures at various points in the system and output
them onto an electrical temperature monitor (21). Liquid and gaseous samples are taken at ever one of the 6
stages via sample ports (L1-L6 &G1-G6) and tested with a Refractometer to calculate the density and
eventually the composition of the samples.
Table 1: Binary Distillation Apparatus Summary (For Figure 5)
Component No.
Apparatus Component
Manufacturer
Description
Notes/Safety
1

Water Connection for


Apparatus

ChE Unit Ops

Water supplied by lab

Water Supply Valve

MCD

Used to load water into Storage Tank.

Funnel

Na

13 Gallon Feed Tank

Nalgene

Feed Supply Valve

Nalgene

Three way valve

Swagelok

Used to ease filling of solutions


Used to load 5 mol% ethanol solution
before filling flask
Only open when filling round bottom
flask
Valve is labeled to either drain, fill or
prevent loss

Round Bottom Flask

Na

Valves & Sample Ports

Nalgene

Glass sections of column

Na

10

Cooling water Connection


for Apparatus.

ChE Unit Ops

Cooling water is supplied by lab

11

Cooling Water Supply Valve

Cold Chicago
Faucets

Used to start flow of cooling water


into system.

12

Cold Water Temperature


Gauge

Marsh Instrument
Company

Measures the temperature of the


incoming cooling water.

Range: 0-60 oF, Increments: 1 oF

13

Cooling Water Apparatus


Valve

Cold Chicago
Faucets

Used to start flow of cooling water


into apparatus.

Check for leaks and cracks.


Always open when distillation
column is in operation to supply
ample cold water.

14

Cold Water Rotameter


(Measures in liquid GPM)

Schutte &
Koerting Co.

15

Temperature Gauge

Moeller

16

Cooling Coil

Na

17

Temperature Gauge

Weksler

Used to hold the Methanol-water


solution
Located at different heights along the
column to obtain experimental
samples
Each section at collection point is
pieced together. The top piece
contains the cooling water tubes and
a narrowed opening so that total
reflux can be assumed.

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Measures flow of cooling water into


cooling coil.
(Measures in liquid GPM)
Measures temperature of cooling
water before entering cooling coil in
degrees Celsius.
Coil where heat transfer takes place
between distillate and cooling water
to provide total reflux.
Measures temperature of cooling
water exiting column in degrees

Check for leaks and cracks.


Clean up spills immediately.
Check for leaks and cracks that
could cause malfunctions.
Do not overfill
Check for cracks and overall
structural integrity.
Check for leaks and cracks that
could cause malfunctions.
Check for leaks and cracks that
could cause malfunctions.
Do not heat when empty!!
Ensure flask is cooled before
adding any fluid Look for any
leaks or cracks before adding
solution or heat.
Check for cracks and leaks that
could cause malfunctions.
Examine entire column for any
leaks, cracks or anything that
could fracture structural integrity
Always open when distillation
column is in operation to supply
ample cold water.
Always open when distillation
column is in operation to supply
ample cold water.

Check for leaks and cracks that


could cause malfunction
Check for any leaks or cracks that
could cause malfunctions.
Check for any leaks or cracks that
could cause malfunctions.
Check for any leaks or cracks that
could cause malfunctions.

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18

Cold Water Drain Valve

Cold Chicago
Faucets

19

Heat Controller

Na

20

Heat Supply for Heating


Jacket

Powerstat

21

Digital Temperature Monitor

Monogram

22

Thermocouples

Omega

23

Power switch for heater

Square D Safety
Switch

24

Electric Heating Jacket

Na

Component No.

Celsius.
Allows cooling water to exit system
and drain.
Used to turn on heaters individually
including heating jacket.
Conducts electricity and passes it into
the heating jacket
Displays temperature taken at the
different thermocouples.
Measure temperature at different
stages in distillation column.
Reading outputs on Digital
temperature display
Controls the electricity passing into
the electric heating jacket turning it
either on or off.
Heats the bottom of the distillation
column electrically.

Make sure probes are secure and


allow no leaks to touch them.
Do not turn on unless cold water
is flowing. Monitor temperatures
and adjust as needed.
Very HOT. Exercise extreme
caution during operation.

Table 2: Binary Distillation Thermocouple Summary (For Figure 5)


Apparatus Component
Manufacturer
Description

T1

Round Bottom Flask


Thermocouple

Omega

Measures temperature of solution in


round bottom flask.

T2

Stage 1 Thermocouple

Omega

Measures the temperature at stage 1.

T3

Stage 2 Thermocouple

Omega

Measures the temperature at stage 2.

T4

Stage 3 Thermocouple

Omega

Measures the temperature at stage 3.

T5

Stage 4 Thermocouple

Omega

Measures the temperature at stage 4.

T6

Stage 5 Thermocouple

Omega

Measures the temperature at stage 5.

T7

Stage 6 Thermocouple

Omega

Measures the temperature at stage 6.

T8

Thermocouple above Stage 6

Omega

Measures the temperature above stage


6.

T9

Thermocouple placed before


cooling coil

Omega

Measures the temperature of the


cooling water before it is introduced
into the cooling coil.

Component
No.
G1

Check for any leaks or cracks that


could spill water
Check for any leaks or cracks that
could cause malfunctions.
Examine for loose wires or
malfunction
Check for loose wires or
malfunctions that may be
causedby leaks.

Notes/Safety
Make sure probe is secure and
tube is filled with white oil.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.

Table 3: Binary Distillation Sample Port Summary (For Figure 5)


Manufactur
Apparatus Component
Description
er
Gas Sample Collection Port
for stage 1.

Na

Unit Operations ChE-382 Group No. 3


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Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb

Gas sample collected from the stage 1 sample


plate via a sealed tube and release valve
(collection port).

Spring 2010

Notes/Safety

Keep watch for leaks. Close when no


Keep samples cold by collecting sam
ice. Clean up any spillage immedi

3/11/2010

Binary Distillation

University of Illinois at Chicago

G2

Gas Sample Collection Port


for stage 2.

Na

G3

Gas Sample Collection Port


for stage 3.

Na

G4

Gas Sample Collection Port


for stage 4.

Na

G5

Gas Sample Collection Port


for stage 5.

Na

G6

Gas Sample Collection Port


for stage 6.

Na

L1

Liquid Sample Collection Port


for stage 1.

Na

L2

Liquid Sample Collection Port


for stage 2.

Na

L3

Liquid Sample Collection Port


for stage 3.

Na

L4

Liquid Sample Collection Port


for stage 4.

Na

L5

Liquid Sample Collection Port


for stage 5.

Na

L6

Liquid Sample Collection Port


for stage 6.

Na

Gas sample collected from the stage 2 sample


plate via a sealed tube and release valve
(collection port).
Gas sample collected from the stage 3 sample
plate via a sealed tube and release valve
(collection port).
Gas sample collected from the stage 4 sample
plate via a sealed tube and release valve
(collection port).
Gas sample collected from the stage5 sample
plate via a sealed tube and release valve
(collection port).
Gas sample collected from the stage 6 sample
plate via a sealed tube and release valve
(collection port).
Liquid sample collected from the stage 1 sample
plate via a sealed tube and release valve
(collection port).
Liquid sample collected from the stage 2 sample
plate via a sealed tube and release valve
(collection port).
Liquid sample collected from the stage 3 sample
plate via a sealed tube and release valve
(collection port).
Liquid sample collected from the stage 4 sample
plate via a sealed tube and release valve
(collection port).
Liquid sample collected from the stage5 sample
plate via a sealed tube and release valve
(collection port).
Liquid sample collected from the stage 6 sample
plate via a sealed tube and release valve
(collection port).

Keep watch for leaks. Close when no


Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi
Keep watch for leaks. Close when no
Keep samples cold by collecting sam
ice. Clean up any spillage immedi

4. Materials and Supplies


Material Name

Table 4: Binary Distillation Materials and Supplies Summary


Manufacturer
Description/ Info

Tap Water

Lake Michigan

White Oil

Chevron Superla 5

Used in preparation of
Methanol-water solution.
Used inside the
temperature probe tube
within the round bottom
flask.

Methanol

Aldrich Chemical
Company

99.8% Methanol used to


prepare water-methanol
solution that is then fed
into the distillation
column.

Ice

From Unit OPS Lab

Used to cool test tubes to


ensure vaporization does
not occur in samples.

Micropipette

Na

Used to transfer samples

Unit Operations ChE-382 Group No. 3


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Notes/Safety
Clean up any spillage
immediately.

Clean up any spillage


immediately. Do not ingest
Will vaporize at room
temperature and is toxic.
Do not allow to escape
through top of distillation
column by circulating
ample cold water. Clean
up any spillage
immediately. Do not ingest
Clean up any spillage
immediately. Try to keep
samples cold to ensure
vaporization does not
occur.
Clean up any glass

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University of Illinois at Chicago

Test Tubes

Kimble Glass Company

Refractometer

Bausch & Lomb

Graduated Cylinder

Nalgene

Task wipers

Kimberly Clark
Professional

from apparatus to test


tubes.
Used to hold test solutions
to use in Refractometer for
sample results.
Used in the experiment to
obtain the refractive index
that can be used to
calculate density once
calibrated.
Used to measure Methanol
and H2O to make the
solution
Used to clean equipment
before, during, and after
operations.

breakage immediately if it
occurs.
Clean up any glass
breakage immediately if it
occurs.
Use caution when
handling. Calibrate before
operation.
Clean up any spillage
immediately.
Clean any mess or spillage
promptly.

5. Procedure
Distillation Column Operation:
1. Make a 5 mol% methanol solution by mixing it with water in the 13 gallon feed tank (4)
using graduated cylinders for measurement.
Note: make sure not to over fill the round bottom flask (7). It only needs to be filled
halfway or until the thermocouple (T1) is in contact with the mixture.
2. Pour the methanol-water mixture into the feed container and turn ON the three-way valve
in order to fill up the round bottom flask.
3. Open the cooling water supply valves (11 & 13) to supply cooling water to the distillation
column.
4. Start up the distillation column by turning on the power supply switches (22) to supply
heat to the distillation column.
5. Record the temperature of each of the thermocouples (T1-T9) located throughout the
column by analyzing the digital temperature monitor (21). Also record the readings of
the inlet cooling water temperature gauge (12), the outlet cooling water temperature
gauge (17), the inlet cooling water pressure gauge (15), and the cooling water rotameter
(14).
6. Make sure to collect the samples at each stage via the sample ports (G1-G6 &L1L6) of the distillation column and record the index of refraction by using the
Refractometer.
7. After the distillation process is done, make sure to turn OFF the heater power supply,
and the cooling water supply.
Operating the Bausch & Lomb Abbe-3L Refractometer:
1 Make mixtures from 10% Methanol with water to 100% Methanol in small test tubes
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Binary Distillation

University of Illinois at Chicago

using a pipette.
2 Turn ON the Refractometer and the water heating system.
3 Open the prism assembly and remove the tissue.
4 Use a capillary tube to apply your liquid sample to the prism and close the prism
assembly.
NOTE: Be careful not to let the glass pipette tip touch the prism since this may scratch the
prism glass.
5
6

Adjust the toric lens, so the light shines on the prism and look through the eyepiece.
Analyze the index of refraction of the sample:
a When the index of refraction of your sample is close enough, then you will see
lighter region on the top and darker region on the bottom.
b If you cannot distinguish between these two regions then adjust the compensator
scale dial of the machine and the toric lens until the dark and light region is
completely separated.

Note: it is an iteration process between adjusting the light and the focus wheel located on the
front of the Refractometer.
c Once the clear distinguishable line between dark and light region is seen then
press the momentary contact switch located on the left hand side of the machine
until you see the scale. Then read off the index of refraction by looking at the
top scale and the refined bottom scale.
7 After you have noted down the index of refraction, record the temperature by
reading the temperature scale.
8 Make sure to clean the prism after testing each sample with a solvent and dabbing it with
tissue.

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Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb

Spring 2010

3/11/2010

Binary Distillation

University of Illinois at Chicago

8. Error Analysis
Component

Table 5: Sources of Uncertainty for Binary Distillation Lab


Manufacturer
Uncertainty Expected

100 mL Graduated Cylinder

Nalgene

0.5mL

Electronic Balance

Denver Instrument Co.

0.01g

Temperature Gauges

Weksler
&
Moeller

1 oF

Digital Temperature Monitor

Monogram

0.1 oC

Bausch & Lomb

0.0001

Refractometer

Description

The 100mL graduated cylinder measures


liquid in increments of 1mL. The lines can
be accurately read to within 0.5mL
Via the manufactures website, the scale
used in this experiment has an associated
uncertainty of 0.01g
The temperature gauges measure in
increments of 2 oF. By dividing the
increments by 2 the expected uncertainty
can be projected to be 1 oF.
The temperature monitor measures in
increments of 0.1 oC. The readings are
accurate when the column reaches steady
state and according to the manufacturers
website, are accurate to 0.1 oC.
The Refractometer measures the refractive
index of a mixture in increments of 0.0002.
However, the values can be read accurately
to the nearest 0.0001.

Listed above are components of the binary distillation lab whose specific uncertainties would
directly affect our recoded data. If these uncertainties were to occur, they would affect our
overall results by adding specific uncertainties to them.

9. References
1. Wankat, Phillip C.; Separation Process Engineering, second edition, Prentice Hall,
2007
2. R. Bird, W. Stewart, E. Lightfoot. Transport Phenomena. Wiley, 2006
3. Towler, G. and Sinnott, R., Chemical Engineering Design: Principles. BH, 2008
4. W. McCabe, J. Smith, and P. Harriot, Unit Operations of Chemical Engineering. 7th
ed. McGraw-Hill, 2005.

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Binary Distillation

University of Illinois at Chicago

5. M. J. Moran, H. N. Shapiro, Fundamentals of Engineering Thermodynamics. 5th ed.


Wiley, 2004
6. Edited by Don Green; John Perrys Chemical engineering Handbook, seventh edition,
McGraw-Hill, New York, 1997
7. Dean, John A., Lange's Handbook of Chemistry, 15th edition. New York, NY: John
Wiley & Sons, Inc., 1998.
8.

Felder, Richard M., and Ronald W. Rousseau. Elementary Principles of Chemical


Processes. 3rd ed. New York, NY: John Wiley & Sons, Inc., 2000.

9. Bennett C.O., Myers J.E., Momentum, Heat, and Mass transfer. 3 rd edition New York.
McGraw-Hill, 1982.
10. Wikipedia: http://en.wikipedia.org/wiki/Distillation
11. Website: http://lorien.ncl.ac.uk/ming/distil/distil0.htm

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