HEAT AND MASS TRANSFER LAB (DRAFT)

STEADY STATE MULTI-STAGE DISTILATION

Before performing this experiment, all students in the lab group should review this protocol in its entirety and also
the references provided. In addition to the measurement detailed out in the procedures, research and report other
data necessary to meet the experimental objectives in the prelab report.

Objectives
1.

To investigate steady state continuous distillation of a binary mixture with reflux.

2.

To determine the overall efficiency of separation by the distillation Column.

3.

Perform a stage by stage analysis of separation process in the Distillation Column.

Equipment Required
1.

Armfiled UOP3CC Continous Distillation Column

2.

Binary solution of composition 50 mol % ethanol/ 50 mol % water

3.

1 - 250 ml measuring cylinder graduated in mL.

4.

1 - stop watch

5.

1 -refractometer

Task
As part of your Prelab Report for this experiments, the Group should:
1.

calculate the volumes of ethanol and water required to prepare 10 Liters of binary solution
with a composition of 50 mole percent of ethanol and 50 mole percent of water.

2.

research and report the Vapor Liquid Equilibrium (VLE) data for ethanol/water system.

3.

plot a VLE curve for an ethanol/water binary system (molar composition) at 1 atm.

4.

Derive a general formulae relating the volumes of ethanol to water require to make up any
molar composition of an ethanol/water binary mixture.

5.

Research the McCabe-Thiele Method, the Lewis-Sorel Method and the Fenske Formula.

EXPERIMENTS

A.
1.

Refractometer Calibration Curve

Fill the 11 sample bottles with exact volumes of water and ethanol required to make 10mL
of a binary mixtures of different molar composition. Vary the volumes of ethanol in each
bottle from 0 mL to 10mL.

2.

Shake all the bottles vigorously for thorough mixing.

3.

Use the refractometer, to determine and record the refractive index (R.I.) of each sample.

Plot a calibration curve of the Molar Composition of Ethanol (xA) vs. Refractive index (R.I).

B.

Calibration curve for the feed pump

1.

Filled Feed Tank A with water to about 90% of its volume. Pass the feed tube over rollers
of the peristaltic pump and clamp it.
Turn on the Control console and turn the pump on.
Set the pump control dial to the 5-mark and allow the water flow to equilibrate.
Collect about 20 mL of water and note the time of collection noted.
Repeat the timed collection and determine the average discharge rate.
Repeat steps 3 through 5 for different pump control dial settings.

2.
3.
4.
5.
6.

Plot a calibration Curve of Pump Dial Settings versus Average Volumetric Flow Rate.

MULTISTAGE DISTILLATION

Armfiled UOP3CC Distillation Equipment Start up Procedure

The distillation the equipment should be turn on or off under the guidance of the Lab Manager.
1. Make up 10 liters of a mixture of 50 mole percent ethanol and 50 mole percent water.
Show all calculations to determine the volumes of ethanol and water used.
2. Ensure all valves on the equipment are closed.
3. Locate and open the filler cap on top of the reboiler. Load the 10 liters of prepared feed
mixture (the liquid to be distilled) directly into the reboiler. Make sure the filler cap is firmly
replaced.
4. Open valve V5 and set the cooling water flow rate on FI1 to approximately 3 liters/min.
5. Turn on the power to the control console.
6. Open valve V10 on the reflux pipe.
7. Switch off the reflux timer on the console so that the column operates at total reflux.
8. Set the temperature selector switch to T9 (the temperature in the reboiler).
9. Turn on the power switch of the heating element. (A red lamp will illuminate indicating the heating
element is on).
C.

Multistage Batch Distillation

Objectives: To determine the overall separation efficiency of the Distillation column

Procedure
1.

Perform steps 1 to 9 of the Equipment Start Up Procedure.

2.

Set the heat controller high to bring the binary mixture to a boil then reduce heat as reflux is
introduced to give a steady bubbling on all tray at total reflux.

3.

Leave the apparatus for at least 30 minutes so the system will reach equilibrium.

4.

Measure the boil-up rate by performing a timed volume collection:

Operate valve V3 so that all the condensate is diverted into a measuring cylinder.
First take a small discarding sample (about 5 to 10 ml) of condensate in beaker and
discard in the RECYCLE BOTTLE.

Use a stopwatch to measure the time required to collect a set volume of

condensate.
Ensure equilibrium conditions in the column are not disrupted by maintaining a
liquid level in the condensate feeding pipe. When taking a sample, partially open
valve V3 and drain the condensate (in a separate measuring cylinder) from the reflux
system until a steady flow is obtained. (Ensure that liquid remains in the flexible
connecting tube to prevent vapour from escaping.)
Start sample collection and timing at the same time, and collect a sizeable amount.

5.

Repeat the timed collection of condensate three times and take an average value to determine
the boil-up rate.

6.

Measure and record the refractive index for the overhead samples and determine the
condensate composition (xD).

7.

Following a similar procedure, take a sample of the bottom through valve V2.
CAUTION! THIS SAMPLE WILL BE HOT!

8.

Record the refractive index, and determine the bottom fraction composition (xW).

9.

Repeat this procedure every ten minutes until 3 samples of overhead and bottom are obtained.

10.

Record the temperatures T8 and T1 and calculate the average column temperature.

11.

Record the temperatures T11 and T12 and determine the condenser load.

Use the Refractometer Calibration Curve from Experiment A to determine all sample composition.
As part of your report for this experiment:
1.

Note the number of actual plates of separation in the column.

2.

Determine the number of theoretical stage of separation:

i.

using the McCabe Thiele Method (graphical Method).

ii.

using the Fenske Formula.

iii.

by a stage-by-stage analysis of the separation using the Lewis-Sorel Method.

iv.

Determine the overall efficiency of separation by each of these method.

D.

Steady State Multistage Continuous Distillation With Reflux

Objectives: To determine the overall separation efficiency of the Distillation column

Procedure
1.

Perform steps 1 to 9 of the Equipment Start Up Procedure.

2.

Ensure the reflux timer on the console is switched off so that the column operates at total
reflux.

3.

Connect the feed tube to the column at the mid-point (onto tray 5). Set the feed flow to 2
litres/hr (Using the feed pump calibration graph). Turn off the Feed Pump.

4.

On the control panel turn the power controller for the reboiler heating element fully anticlockwise and Turn on the power switch of the heating element. A red lamp will illuminate
indicating the heating element is on. Turn the power controller clockwise until a reading of
approximately 1.5 kW is obtained on the digital wattmeter. The contents of the reboiler will
begin to warm up and this can be observed on the temperature readout for T9.

5.

Eventually, vapor will begin to rise up the column and the progress of this can be observed
by the increasing temperature readouts when the temperature selector is set on T8, T7, T6,
T5, T4, T3, T2 and T1.
The vapor will be condensed and reappear as droplets into the glass walled distillate receiver
vessel. The distillate will build up a small level in the receiver and eventually overflow to
the reflux regulator valve. The cooled distillate will return to the top of the column and
cascade down the trays forming liquid level on each trays and bubbling of vapor through
the liquid.
The system will have reached an equilibrium condition when the temperatures T1, T2, T3,
T4, T5, T6, T7 and T8 have reached an average steady temperature (but note cycling due to
the intermittent reflux).

6.

Before turning the reflux switch on, set the reflux ratio to 5:1. This means 5 sec condensed
distillate will return back to the column and 1 sec to top product receiver. On the Reflux
Controller LCD screen, C- means back to column and C+ means to top product receiver.
When this is done, switch the reflux valve on (on the control panel). You should now hear
a click, meaning the reflux valve is working. You should also see condensed vapor flowing
to the top product receiver.

7.

When the column has stabilized at total reflux (it takes 15 to 30 minutes), the Feed Pump
and the reflux timer can be started at the same time.

8.

As the flow into the column becomes established, more vapor will rise up the column and
appear as condensate in the distillate receiver, allow this to flow to the top product receiver.

9.

After pumping approximately 3 liters of Feed, take a discarding sample of about 5-10 mL
of the overheads through valve V3. Be careful never to drain the condensate return line ie.
partially open valve V3 to leave a small amount of liquid in the line all the time. Take a
further four samples. Discard the discarding sample in a safe manner.

10.

Take a condensate sample. Start collection and timing at the same time, and collect a
sizeable amount.

11.

In a similar manner and preferably at the same time as step 11, take a timed sample of
the bottom through valve V2.
CAUTION! THIS SAMPLE WILL BE HOT.

12.

Record the refractive index and composition for the condensate (xD) and the bottom (xW).

13.

Draw samples from each stage. Determine the Refractive index and compositions of each
sample.

14.

Record the temperature of the liquid on each stage

15.

Repeat the sample taking (steps 10-13) three more times at 10 15 minutes time intervals
before feed runs out.

16.

Record the temperatures T11 and T12.

17.

Record the feed temperature T14 and temperature of liquid from the top stages of the
column, T10.

As part of your report for this experiment:

1.

Perform total material and component balances around the whole column and the top and
bottoms parts to determine the Feed, Condensate and Bottoms.

2.

Use the McCabe Thiele Method (graphical Method) to analyze the operations of the
column.

3.

By performing a stage-by-stage analysis of the separation using the Lewis-Sorel Method.

4.

Use temperatures T11 and T12 and to determine the condenser load.

5.

Use the feed temperature T14 and temperature of liquid from the top stages of the column,
T10, and determine how much heat was used to heat and vaporize the feed.

RESULTS AND DATA ANALYSIS

In addition to all measurements detailed in the procedures, research and report:
1. Molecular weights of ethanol and water.
2. Refractive indices of ethanol and water at room temperature.
3. Densities of ethanol and water at room ambient temperature.
1. Number of actual stages in the distillation column.
2. Top temperature (C)
3. Bottom temperature (C).

Use the refractometer and the calibration curve to obtain the RI and compositions of all samples obtained
during in the experiments.
Column and process temperatures and reboiler power can be obtained from the control console.
Determine and report the compositions of the all Feed (xF), Condensate (xD) and Bottoms (xB)
products.

Discussions/ Conclusion
Is there any relationship between boil-up rate and column efficiency?
Compare your result from the McCabe-Thiele Method and the Lewis-Sorel Method.

Useful Reference
1)

Geankoplis, Christie J. Transport Processes and Separation Process Principles: (includes

Unit Operations). Prentice Hall Professional Technical Reference, 2003. Upper Saddle
River, NJ 07458.

2)

McGraw-Hill Book Company. Chemical Engineers Handbook (5th. Ed.). Perry H. R.

(Consultant) and Chilton H. C. (Senior Advisor).

3)

Armfield Distillation Column UOP3CC Instruction Manual.

Useful Information