Manual for continuous distillation

1. Week 1:

Objectives:
Run the column at total reflux.
When steady state is reached, take the sample from the top and
bottom of the column in order to determine the overall efficiency.
Based on the overall efficiency, draw the quasi equilibrium curve.
Compare the tray numbers you get from the quasi equilibrium line
with the actual tray numbers.
Take the samples from consecutive trays to determine the local
efficiency.

Operation procedure:

Preparation for Start-up:

Key purposes:

Get familiar with the system; locations of the valves and sample
taps

Check the liquid level in the reboiler

Check the composition in the reboiler and feed tank

Turn the Siemens system on

Check if the valves are in the correct position

1. Using the sight-glass on the reboiler to assess its level of the liquid
(in the range of around 70%).
2. Prepare to mix the contents of the reboiler.
a. Close the red gauge valve on the bottoms line.(see graph
below)
b. Open the green valve on the same line just after it exits
the reboiler.
Follow the line down to the bottom of the reboiler. Open the orange ball

valve and make sure that the blue ball valve on the sample port is closed
3. Ask the TA/Lab Assistant to turn on the computer system hooked
to the East column.
4. Using the computer control system, turn on the reboiler-mixing
pump on the 1st floor, as shown below to mix the contents of the
reboiler. Let mix for at least twenty minutes.
5. While you are waiting, check that the manual by-pass valves are
closed.
a. Refluxred valve parallel to the Reflux control valve
b. Distillatered valve parallel to the Distillate control
c. Bottomsblue valve parallel to the Bottoms control
d. Waterblue valve parallel to the Water control valve

Red gauge valve

on Bottoms line
Blue ball valve on
line

exiting

reboiler

Orange valve at
bottom

of

reboiler open
while mixing

Figure 1. East Column Reboiler Pumping Line

Figure 2. East column second floor control valves

Start up:
1. Ensure that the reboiler has enough material and then turn on the air
for the 1st floor by manually opening the air valve fully. The exact
position of the valve is A of the graph shown below. Air is needed to
operate pneumatic control valves.
2. Turn the water on for the 1st floor by manually opening the water
valve fully. The exact position of the valve is C in the picture below.
Water is needed for cooling purposes. Water valves by convention are
blue in color.
3. Kindly note the sequence of turning on the utilities, it is air first (no
cost) followed by water (somewhat expensive) followed by steam
(highly expensive). The sequence will be exactly reversed while
turning them off. The rationale is to cut-off the steam and save the
operating cost as much as possible.
4. Ask the Lab Assistant/TA to purge the steam lines using the steam
purge valve located on the 1st floor. While the lines are being purged,
the students should have fingers in their ears and should not be
directly facing the outlet of the purge line. The Lab Assistant/TA
should have ear plugs. The ear plugs should necessarily be discarded
after one use.
5. Repeat steps 1 and 2 on 2nd floor. i.e. turn on the air for the 2nd floor
by manually opening the air valve fully. The exact position of the

valve is B. Also, turn on the water for the 2nd floor by manually
opening the water valve fully. This valve is a large blue valve located
at the base of the water rotameter, which is D shown in the picture.
6. Then go to the Control Room. One of the computer systems is hooked
to the West Column. The system would have already been made on by
the Lab Assistant/TA. The computer screen will indicate values of
different process parameters like temperature, pressure and flow rates
as well as the positioning of different valves. Note that the values of
some of the parameters might not be correctly shown on the screen
due to some or the other reason and typically such values will be
grayed out. Set the Steam/PID on the screen. Usually 40% is a good
start for batch column. You will slowly see a rise in the temperature of
the liquid in the reboiler and the pressure. You should see the boiling
of the liquid in some time. Allow a stable level to be attained in the
sight glass. Set the Reflux/PID to a 100%. Now, it essentially
means that you are operating the column at total reflux.
In case, you see the column flooding meaning the sight glass getting
overfilled, turning on the Reflux Pump momentarily helps it to get
stable. When the Reflux Pump turns on, it will be indicated in green.
Reducing the % in the Steam/PID also helps to lower down the
level of the material in the sight glass.
7. After the level of the material in the stand pipe is at a fairly stable for

some time, check if the system has attained steady state or not. This
can be done by measuring the composition of one of the streams
(reflux is the easiest because it is located on the second floor) as a
function of time. When the composition changes by less than 5% with
time, the system can be considered in a steady state condition. The
reflux sample port is located on the second floor.

B
A

A- Air supply on the first floor

B- Air supply on the second floor
C- Cooling water on the first floor
D- Cooling water on the second floor

Shutting Down

1. As mentioned before, the utilities will be turned off exactly in the

reverse order meaning steam first, then water and lastly air. Use the
computer system to close the Steam control valve. To close the steam
valve, click on the display box labeled STEAM/PID located above the
valve symbol on the reflux line. Click on the box to the right of MAN.
A small window will pop up. Change the opening of the valve to 0 and

click OK.
2. Turn off the reboiler mixing pump (EBTP/PUMP):
a. To turn off the reboiler-mixing pump: click on Bottoms/PUMP or
the pump icon; if not yet in manual mode, click on Manual; click
Stop and close the window.
3. With the reflux control valve (Reflux/PID) fully open, use the reflux
pump (Reflux/PUMP) to drain the standpipe. Turn pump off.
a. To open the reflux valve: Click on the display box labeled
Reflux/PID located above the valve symbol on the reflux line. Click
on the box to the right of MAN. A small window will pop up.
Change the opening of the valve to 100 and click OK.
4. Open the red reflux valve (also serves as a manual bypass valve) (see
Figure 1).
5. Close manual valves associated with the distillate tank (Figure 3).
6. Turn off the water and air valves by manually turning them fully in the
clockwise direction on both floors.

Figure 3. Tanks on the first floor.

Calculation:

Overall efficiency can be calculated by comparing the actual number of

plates in the column with the number obtained from McCabe-Thiele
diagram when the column operates at total reflux. Local or point
efficiencies can be calculated by measuring the compositions of the liquid
streams corresponding to two successive plates. The local efficiency is
typically close to the overall efficiency.

Eoverall =

Ntheoretical
100%
Nactual

The theoretical tray numbers can be obtained as follows:

Generate the equilibrium curve with relative volatility;
Draw horizontal and vertical lines between the equilibrium line and
y=x from the top product composition to bottom product composition;
Tray numbers can be counted in the graph.
An example drawing of the procedure is shown in Fig 1.
From this graph,
Ntheoretical = 7 1 = 6
Assuming the actual tray number is 12,
Eoverall =

Ntheoretical
6
100% =
= 54.5%
Nactual
12 1

1.0
2
3

0.6

yA

equilibrium line

0.8

0.4
6

0.2

0.0
0.0

xB0.2

0.4

xA

0.6

0.8

xD

1.0

Fig 1. An illustration of the way to get theoretical tray numbers

Given the analytical equation of equilibrium line, y = f(x), and the

overall efficiency of the column, Eoverall , we can get the analytical
expression of quasi equilibrium line as blow:
y = x + Eoverall (f(x) x)
Compare the tray numbers getting between the quasi equilibrium line and
the y=x to the actual numbers to verify the validation of the
McCabe-Thiele diagram. The way to get quasi equilibrium line is shown
in Fig 2. In Fig 2, b represents the driving force at a certain tray if at
ideal case, a is the driving force in reality in the column we run.

1.0
0.8

equilibrium line

yA

0.6

0.4

a/b=Eoverall

0.2

quasi equilibrium line

0.0
0.0

0.2

0.4

xA

0.6

0.8

Fig 2. An illustration of the way to get quasi equilibrium line

1.0

1.0
0.8

equilibrium line

yA

0.6
0.4
quasi equilibrium line

0.2
0.0
0.0

xB

0.2

0.4

xA

0.6

0.8

xD

1.0

Fig 3. An illustration of the way to count the number of trays

In Fig 3, the tray numbers getting from the quasi equilibrium line is 10
and the actual tray numbers is 11.
Error =

11 10
100% = 9.1%
11

By taking the sample from successive trays, the local efficiency can be
worked out as follows:
Elocal =

yn yn+1 xn1 xn
=
yn yn+1
yn x n

Fig 4 is a graphical description.

1
equilibrium line

yA

yn
yn
yn+1

y=x

0
0

xn xn-1

xA

Fig 4. An illustration of the way to get local efficiency

2. Week 2:

Run the column at different reflux ratios.

Study the effect of reflux ratio on the concentrations of top and
bottom product.

Operation procedure:

From week 2 onwards, it is suggested to check if the reboiler has enough

material from the control panel before starting the experiment. If the
liquid level in the reboiler is less than 15 in, the liquid in the distillate
tank should be pumped back to the. To pump the distillate back, you need
to follow the procedure below. First open two valves located below the
distillate tank, which are shown in graph E.

Then open the bypass valve

which is indicated on graph C. Finally open the pump below the reboiler
on graph F. When you pump the liquid back to the reboiler, make sure
someone checks the level in the distillate tank, as you may run the risk of
burning the pump if the distillate tank is pump to empty.

The general start up procedure followed is the same as the first week
during all the three weeks, so repeat procedure 1~7 at first for week 2 and
week 3. Open the valve beside the rotameter on B to change the distillate
flow rate in order to change the reflux ratio. The distillate will go through
the rotameter on the 2nd floor down to the tank located on the 1st floor,
which is shown in graph E.

Notes: All composition measurements are done with a Perkin Elmer Gas
Chromatography instrument in the Lab. Get help from the lab assistant on
using it.

Shutting Down
Turn off the valve for distillate first. Then shut down the steam on the
control panel, which means set the PID of steam to 0%. Wait for 1~2min,
as after shutting off the stream, the vapor may still go to the top and that
means the water is still needed to condense the top product. Then close
the air and water valves on the first and second floor, just like the shutting
down procedure for the first week.

Reflux
rotameter

Reflux sampling port

Distillate rotameter

Sight glass

Bypass valve

Bottom product sampling port

2
1

F
A- Reflux rotameter
B- Distillate rotameter
C- East column 1st floor reboiler
D- East column second floor control valves.

E- Distillate tank for east column

F- Control panel overview of the east column

3. Week 3:
Run the column at different reflux ratios.
If there is still time left, run the column with a reflux ratio smaller
than the minimum reflux ratio.

GC (gas chromatography)

For our GC system, the absolute value of the peak area will vary
a lot even if the same sample is injected for several times, which
can be observed with the error bar in the graph. For this graph,
four standard samples are tested and each concentration is
calibrated for three times. The absolute peak area and peak area
percentage is taken out to draw the curve.
In the graph, the black points are absolute value of the peak
area of ethanol, while the blue points are the peak area of
ethanol over the total area, which is a relative number. The error
bar for the absolute area is huge, especially for the mole fraction
around 0.6, but for the relative area, the error bar can be barely
seen, indicating a more reliable measurement for our GC
system.

Equation

y = a + b*x

Weight

Instrumental

Peak area (V*s)

Residual Sum of
Squares

1.5

Adj. R-Square

150

18.80314
0.98832
Value
Intercept

Mean

1.0

Slope

Standard Error

-316738.0310

42671.23728

2.11196E6

43147.6728

100

absolute area
relative area

0.5

Equation

y = a + b*x

Weight

Instrumental

50

Residual Sum of 6921.93153

Squares
0.98842
Adj. R-Square
Value

0.0
0.00

Mean

0.25

0.50

Standard Error

Intercept

-21.25416

0.09766

Slope

116.4014

0.12339

0.75

Mole fraction

1.00

0
1.25

For this method, there is not much calculation going on. The
students need to calibrate the curve with relative peak area as
the graph above. As the peak area percentage of a same sample
will not vary much for different runs, the students just need to
run each concentration once. After getting the calibration curve,
they can use this curve to get their mole fraction directly from
the relative peak area for the three-week experiment.

Peak area percentage(%)

2.0