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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 p. 1 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

Table of Contents
1. WP&C .................................................................................................................................................. 2
1. Introduction ......................................................................................................................................... 4
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?

Unit Operations ChE-382 Group No. 3 p. 2 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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.

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

Unit Operations ChE-382 Group No. 3 p. 3 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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.

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

Unit Operations ChE-382 Group No. 3 p. 4 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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

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.

= ( + ) (1)

Where,

Unit Operations ChE-382 Group No. 3 p. 5 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

[=] Vapor pressure of mixture [kPa]

[=] Vapor pressure of component a [kPa]

[=] Vapor pressure of component b [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.


= (2)

Where:

[=] 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]

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

Unit Operations ChE-382 Group No. 3 p. 6 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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.

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.

Unit Operations ChE-382 Group No. 3 p. 7 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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).

Figure 3: This shows a simple McCabe-Thiele diagram. The number of steps corresponds to the
number of trays needed for a given mixture.

Unit Operations ChE-382 Group No. 3 p. 8 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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 boil-

up, 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.

Unit Operations ChE-382 Group No. 3 p. 9 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
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

Unit Operations ChE-382 Group No. 3 p. 10 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

liquid, we change the number of theoretical plates necessary for a given separation. The q

(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:


= (3)

Where:

[=] quality of the feed (dimensionless)

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

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:


=( ) + (4)
1 1

Where:

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

q [=] quality of the feed (dimensionless)

Unit Operations ChE-382 Group No. 3 p. 11 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

x [= ] liquid mole fraction of methanol (dimensionless)

ZF [=] mole fraction of methanol in feed (dimensionless)

The top operating line is defined as

0 0

= + (1 ) (5)
(1+ 0 ) 1+ 0

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 multi-

component 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.

Unit Operations ChE-382 Group No. 3 p. 12 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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.

3. Apparatus

Unit Operations ChE-382 Group No. 3 p. 13 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
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.

Unit Operations ChE-382 Group No. 3 p. 14 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

Table 1: Binary Distillation Apparatus Summary (For Figure 5)


Component No. Apparatus Component Manufacturer Description Notes/Safety
Water Connection for Check for leaks and cracks.
1 ChE Unit Ops Water supplied by lab
Apparatus Clean up spills immediately.
Check for leaks and cracks that
2 Water Supply Valve MCD Used to load water into Storage Tank.
could cause malfunctions.
3 Funnel Na Used to ease filling of solutions Do not overfill
Used to load 5 mol% ethanol solution Check for cracks and overall
4 13 Gallon Feed Tank Nalgene
before filling flask structural integrity.
Only open when filling round bottom Check for leaks and cracks that
5 Feed Supply Valve Nalgene
flask could cause malfunctions.
Valve is labeled to either drain, fill or Check for leaks and cracks that
6 Three way valve Swagelok
prevent loss could cause malfunctions.
Do not heat when empty!!
Ensure flask is cooled before
Used to hold the Methanol-water
7 Round Bottom Flask Na adding any fluid Look for any
solution
leaks or cracks before adding
solution or heat.
Located at different heights along the
Check for cracks and leaks that
8 Valves & Sample Ports Nalgene column to obtain experimental
could cause malfunctions.
samples
Each section at collection point is
pieced together. The top piece Examine entire column for any
9 Glass sections of column Na contains the cooling water tubes and a leaks, cracks or anything that
narrowed opening so that total reflux could fracture structural integrity
can be assumed.
Always open when distillation
Cooling water Connection
10 ChE Unit Ops Cooling water is supplied by lab column is in operation to supply
for Apparatus.
ample cold water.
Always open when distillation
Cold Chicago Used to start flow of cooling water
11 Cooling Water Supply Valve column is in operation to supply
Faucets into system.
ample cold water.
Cold Water Temperature Marsh Instrument Measures the temperature of the
Range: 0-60 oF, Increments: 1 oF
12 Gauge Company incoming cooling water.

Check for leaks and cracks.


Cooling Water Apparatus Cold Chicago Used to start flow of cooling water Always open when distillation
13
Valve Faucets into apparatus. column is in operation to supply
ample cold water.
Measures flow of cooling water into
Cold Water Rotameter Schutte & Check for leaks and cracks that
14 cooling coil.
(Measures in liquid GPM) Koerting Co. could cause malfunction
(Measures in liquid GPM)
Measures temperature of cooling
Check for any leaks or cracks that
15 Temperature Gauge Moeller water before entering cooling coil in
could cause malfunctions.
degrees Celsius.
Coil where heat transfer takes place
Check for any leaks or cracks that
16 Cooling Coil Na between distillate and cooling water
could cause malfunctions.
to provide total reflux.
Measures temperature of cooling
Check for any leaks or cracks that
17 Temperature Gauge Weksler water exiting column in degrees
could cause malfunctions.
Celsius.
Cold Chicago Allows cooling water to exit system Check for any leaks or cracks that
18 Cold Water Drain Valve
Faucets and drain. could spill water
Used to turn on heaters individually Check for any leaks or cracks that
19 Heat Controller Na
including heating jacket. could cause malfunctions.
Heat Supply for Heating Conducts electricity and passes it into Examine for loose wires or
20 Powerstat
Jacket the heating jacket malfunction

Unit Operations ChE-382 Group No. 3 p. 15 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

Check for loose wires or


Displays temperature taken at the
21 Digital Temperature Monitor Monogram malfunctions that may be
different thermocouples.
causedby leaks.
Measure temperature at different
stages in distillation column. Make sure probes are secure and
22 Thermocouples Omega
Reading outputs on Digital allow no leaks to touch them.
temperature display
Controls the electricity passing into
Square D Safety Do not turn on unless cold water
Power switch for heater the electric heating jacket turning it
23 Switch is flowing. Monitor temperatures
either on or off. and adjust as needed.

Heats the bottom of the distillation


Electric Heating Jacket Na Very HOT. Exercise extreme
24 column electrically.
caution during operation.

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


Component No. Apparatus Component Manufacturer Description Notes/Safety
Round Bottom Flask Measures temperature of solution in Make sure probe is secure and
T1 Omega
Thermocouple round bottom flask. tube is filled with white oil.
Pay close attention to
Stage 1 Thermocouple Omega Measures the temperature at stage 1. temperature so column does not
T2
overheat.

Pay close attention to


Stage 2 Thermocouple Omega Measures the temperature at stage 2. temperature so column does not
T3
overheat.

Pay close attention to


Stage 3 Thermocouple Omega Measures the temperature at stage 3. temperature so column does not
T4
overheat.

Pay close attention to


Stage 4 Thermocouple Omega Measures the temperature at stage 4. temperature so column does not
T5
overheat.

Pay close attention to


Stage 5 Thermocouple Omega Measures the temperature at stage 5. temperature so column does not
T6
overheat.

Pay close attention to


Stage 6 Thermocouple Omega Measures the temperature at stage 6. temperature so column does not
T7
overheat.

Pay close attention to


Measures the temperature above stage
Thermocouple above Stage 6 Omega temperature so column does not
T8 6.
overheat.

Measures the temperature of the Pay close attention to


Thermocouple placed before
Omega cooling water before it is introduced temperature so column does not
T9 cooling coil
into the cooling coil. overheat.

Unit Operations ChE-382 Group No. 3 p. 16 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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


Component Manufactur
Apparatus Component Description Notes/Safety
No. er
Gas sample collected from the stage 1 sample Keep watch for leaks. Close when not in use.
Gas Sample Collection Port
G1 Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
for stage 1.
(collection port). ice. Clean up any spillage immediately.
Gas sample collected from the stage 2 sample Keep watch for leaks. Close when not in use.
Gas Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
G2 for stage 2.
(collection port). ice. Clean up any spillage immediately.

Gas sample collected from the stage 3 sample Keep watch for leaks. Close when not in use.
Gas Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
G3 for stage 3.
(collection port). ice. Clean up any spillage immediately.

Gas sample collected from the stage 4 sample Keep watch for leaks. Close when not in use.
Gas Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
G4 for stage 4.
(collection port). ice. Clean up any spillage immediately.

Gas sample collected from the stage5 sample Keep watch for leaks. Close when not in use.
Gas Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
G5 for stage 5.
(collection port). ice. Clean up any spillage immediately.

Gas sample collected from the stage 6 sample Keep watch for leaks. Close when not in use.
Gas Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
G6 for stage 6.
(collection port). ice. Clean up any spillage immediately.

Keep watch for leaks. Close when not in use.


Liquid Sample Collection Port Liquid sample collected from the stage 1 sample
Na Keep samples cold by collecting samples with
L1 for stage 1. plate via a sealed tube and release valve
ice. Clean up any spillage immediately.
(collection port).

Liquid sample collected from the stage 2 sample Keep watch for leaks. Close when not in use.
Liquid Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
L2 for stage 2.
(collection port). ice. Clean up any spillage immediately.

Liquid sample collected from the stage 3 sample Keep watch for leaks. Close when not in use.
Liquid Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
L3 for stage 3.
(collection port). ice. Clean up any spillage immediately.

Liquid sample collected from the stage 4 sample Keep watch for leaks. Close when not in use.
Liquid Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
L4 for stage 4.
(collection port). ice. Clean up any spillage immediately.

Liquid sample collected from the stage5 sample Keep watch for leaks. Close when not in use.
Liquid Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
L5 for stage 5.
(collection port). ice. Clean up any spillage immediately.

Liquid sample collected from the stage 6 sample Keep watch for leaks. Close when not in use.
Liquid Sample Collection Port
Na plate via a sealed tube and release valve Keep samples cold by collecting samples with
L6 for stage 6.
(collection port). ice. Clean up any spillage immediately.

Unit Operations ChE-382 Group No. 3 p. 17 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

4. Materials and Supplies

Table 4: Binary Distillation Materials and Supplies Summary


Material Name
Manufacturer Description/ Info Notes/Safety
Used in preparation of Clean up any spillage
Tap Water Lake Michigan
Methanol-water solution. immediately.
Used inside the
temperature probe tube Clean up any spillage
White Oil Chevron Superla 5
within the round bottom immediately. Do not ingest
flask.
Will vaporize at room
temperature and is toxic.
99.8% Methanol used to Do not allow to escape
Aldrich Chemical prepare water-methanol through top of distillation
Methanol
Company solution that is then fed column by circulating
into the distillation column. ample cold water. Clean
up any spillage
immediately. Do not ingest
Clean up any spillage
Used to cool test tubes to immediately. Try to keep
Ice From Unit OPS Lab ensure vaporization does samples cold to ensure
not occur in samples. vaporization does not
occur.
Used to transfer samples
Clean up any glass
Na from apparatus to test
Micropipette breakage immediately if it
tubes. occurs.

Used to hold test solutions


Clean up any glass
Kimble Glass Company to use in Refractometer for
Test Tubes breakage immediately if it
sample results. occurs.

Used in the experiment to


obtain the refractive index Use caution when
Refractometer Bausch & Lomb that can be used to handling. Calibrate before
calculate density once operation.
calibrated.
Used to measure Methanol
Nalgene and H2O to make the Clean up any spillage
Graduated Cylinder
solution immediately.

Used to clean equipment


Kimberly Clark
before, during, and after Clean any mess or spillage
Task wipers Professional
operations. promptly.

Unit Operations ChE-382 Group No. 3 p. 18 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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 &L1-
L6) 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
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.

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Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

NOTE: Be careful not to let the glass pipette tip touch the prism since this may scratch the
prism glass.

5. Adjust the toric lens, so the light shines on the prism and look through the eyepiece.

6. 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.

Unit Operations ChE-382 Group No. 3 p. 20 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

8. Error Analysis

Table 5: Sources of Uncertainty for Binary Distillation Lab

Component Manufacturer Uncertainty Expected Description

The 100mL graduated cylinder measures


100 mL Graduated Cylinder Nalgene 0.5mL liquid in increments of 1mL. The lines can
be accurately read to within 0.5mL

Via the manufactures website, the scale


Electronic Balance Denver Instrument Co. 0.01g used in this experiment has an associated
uncertainty of 0.01g

Weksler The temperature gauges measure in


increments of 2 oF. By dividing the
Temperature Gauges & 1 oF
increments by 2 the expected uncertainty
Moeller can be projected to be 1 oF.

The temperature monitor measures in


increments of 0.1 oC. The readings are
Digital Temperature Monitor Monogram 0.1 oC accurate when the column reaches steady
state and according to the manufacturers
website, are accurate to 0.1 oC.

The Refractometer measures the refractive


Refractometer
index of a mixture in increments of 0.0002.
Bausch & Lomb 0.0001
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.

Unit Operations ChE-382 Group No. 3 p. 21 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Binary Distillation University of Illinois at Chicago

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.

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. 3rd 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

Unit Operations ChE-382 Group No. 3 p. 22 Spring 2010 3/11/2010


Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb

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