How to Operate the Rotary Evaporator

in 221 S. Frear

By: August Rothenberger

Contents
Introduction ................................................................................................................................. 2
Parts of the Rotovap ................................................................................................................. 3
Setting up the Rotovap ............................................................................................................ 4
Using the Rotovap...................................................................................................................... 7
Cleaning up the Rotovap ......................................................................................................... 9
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Introduction
A rotary evaporator (Rotovap) is used to remove solvent from a solution—
most commonly to recover a solute or concentrate the solution. The Rotovap
uses reduced pressure to lower the boiling points of common solvents so they
can evaporate without significant heating. The Rotovap should not be used to
remove solvents with a boiling point over 100°C at atmospheric pressure.

The operation of the Rotovap is quite simple; however, care must be taken to
avoid “bumping” in your sample. Bumping occurs when the solvent
evaporates too rapidly, causing the solution to vigorously bubble out of your
sample flask. Bumping can damage the Rotovap and may lead to loss of your
solute. A bump flask will prevent the solvent from entering the Rotovap, but
bumping can be prevented in most cases by closely following the procedure
described in this document.

The operation of the Rotovap will be divided into three phases. First, you will
prepare the Rotovap for use. Second, you will use the Rotovap to remove
solvent from your sample. Third, the Rotovap will be properly cleaned up so
that another lab member can use it. The complete procedure should take
about 30-90 minutes, depending on how much solvent must be removed.

All images were taken by the author and depict the Rotovap in 221 S. Frear.

Warning:
Wear gloves and eye protection at all times when operating the Rotovap.
The machine may have chemical residue on its surface which could cause
bodily harm if contacted.

Wear protective gloves (cold gloves) when handling dry ice. Direct skin
contact with dry ice, even for a short time, could result in frostbite.
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Parts of the Rotovap

15

12
9 10 11

7 6
8
13

5 2
4

3 1
14

1. Power Switch 9. Vent Valve

2. Water Bath 10. Water Condenser
3. Temperature Display 11. Water Intake/Outtake Tubes
4. Height Control Arm 12. Slush Bath
5. Vacuum Pump 13. Stopcock
6. Sample Holder 14. Bump Flask
7. Rotation Dial 15. Pressure Gauge (behind slush
8. Collection Flask bath)
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Setting up the Rotovap

.....................................................................................................................................................................................
Warning: The Rotovap may contain chemical residue. Always wear gloves
and safety glasses when operating.

1. Fill the bath to about 3 inches from

the top with warm water.

...............................................................................................................................................................
2. Turn on the Rotovap by pressing the
power switch.
The Rotovap will power on and
display the temperature of the bath.

...............................................................................................................................................................
3. Set the bath to heat to your desired
temperature using the arrows. 30-
35°C is suitable for most solvents.
The display will blink for a few
seconds at the set temperature, then
will revert to the current bath
temperature

...............................................................................................................................................................
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4. While the bath warms up, connect

one of the water intake tubes to the
faucet. Leave the other in the sink.
Carefully turn on the cold-water
faucet so there is constant flow
through the water condenser.

...............................................................................................................................................................
Warning: Dry ice can damage skin. Wear cold gloves when handling.

5. Gather dry ice for the slush bath. Use

the hammer and screwdriver at the
ice chest to break the ice into chunks
about 2 inches in diameter.

...............................................................................................................................................................
6. Drop one piece of ice into the liquid
(acetone) of the slush bath.
The bath will bubble rapidly as the
temperature of the bath decreases.

...............................................................................................................................................................
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7. One the bubbling has slowed, fill the

bath to the top with dry ice. In order
for the bath to remain at the proper
temperature, at least one piece of dry
ice must be above the level of the
acetone.

...............................................................................................................................................................
8. Attach the bump flask to the joint and
tighten the sample holder. Catch the
lip of the flask with the wire so that is
snug and will rotate with the sample
holder.

...............................................................................................................................................................
9. Attach your sample to the bump
flask and secure it with a joint clip.
The solution should not enter the
neck of the sample flask. Transfer
your solution to a larger flask or
fraction your sample into multiple
flasks if it does.
...............................................................................................................................................................
10. Ensure both the vent valve and the
stopcock are closed. The closed
position is perpendicular to the
outlet direction for both.
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Using the Rotovap

...............................................................................................................................................................
1. Slowly turn the rotation dial to 8. If
the sample is wobbly, cease rotation
and ensure that the bump flask is
snugly held to the sample holder.

...............................................................................................................................................................
Caution: Your sample is at risk of bumping once it is under vacuum. Read
ahead and ensure you are able to recognize and troubleshoot bumping
before proceeding.

2. Turn on the vacuum pump. If you see

vigorous bubbling, open the vent
valve until the bubbles stop. Increase
the rotation speed, then close the
vent valve and resume. If this does
not rectify the issue, consider using a
different method to remove your
solvent.
...............................................................................................................................................................
3. Once the pressure gauge reaches 30
in. Hg, use the height control arm to
lower your sample into the water
bath.

...............................................................................................................................................................
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4. Carefully watch your sample. If

bumping occurs, open the vent valve.
If bumping continues after vacuum is
restored, lift the sample out of the
bath and lower the bath temperature
until the sample no longer bumps
when immersed.
...............................................................................................................................................................
5. When solvent begins to drip from the
water condenser or slush bath at a
regular rate without bumping, you
can leave the sample to evaporate on
its own. Increase the bath
temperature if solvent does not begin
to condense after about 10 minutes.

...............................................................................................................................................................
6. Once solvent has been removed from
the sample to your satisfaction, stop
the rotation of the flask, then use the
height control arm to lift it out of the
water bath.
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Cleaning up the Rotovap

...............................................................................................................................................................
1. Turn off the vacuum pump. Re-
pressurize the Rotovap by opening
the vent valve.
Air will audibly rush into the machine
to re-pressurize it.

...............................................................................................................................................................

Caution: Do not attempt to remove your sample before re-pressurizing. The

sample will be very difficult to remove and you may damage the machine.

2. Remove the joint clip and your

sample by gently pulling it from the
bump flask. Remove the bump flask
by unscrewing the sample holder
until the flask is pushed off. Clean the
bump flask if it was dirtied.

...............................................................................................................................................................
3. Remove the solvent from both
condensers. The ice condenser is
opened using the stopcock and the
water condenser by removing the
clamped collection flask. Return the
collection flask after emptying it.

...............................................................................................................................................................
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4. Turn off the faucet. Remove the

water intake tube and let it drain into
the sink.

...............................................................................................................................................................
5. Turn off the machine. You can leave
the water in the heating bath and dry
ice/acetone in the slush bath. The
Rotovap is now properly cleaned and
ready for another lab member to use.