ANALYTICAL TECHNIQUES

COURSE#509
ROTARY EVAPORATOR
The rotary evaporator (rotovap) can be used to remove low boiling organic chemicals, usually
solvents, from a mixture of compounds. The solvents or low boiling compounds are removed
by a simple distillation at reduced pressure.
The rotation transfers a thin film of the liquid sample to the whole of the inner surface of the
flask, markedly increasing evaporation rate and assisting heat transfer from the heating bath.
The rotating flask and vapour duct have a sealing system which allows operation under
vacuum, further accelerating the evaporation process because of the reduction in boiling point
of the solvent and efficient removal of the vapour. Vacuum operation also permits heat
sensitive materials to be successfully concentrated without degradation.
HOW DOES IT WORK?
The fact that a vacuum is usually applied to the setup means that the boiling points of the
solvents are going to be significantly lower than at ambient pressure. ince the flask is rotated
during the evaporation process, the surface area is larger which increases the evaporation
rate. These two factors combined make it a very useful tool in synthetic chemistry to remove
solvents. !n addition, the need for lower temperatures also avaoids overheating of the target
compounds. "owever, if a aspirator is used, this procedure is not suitable for moisture
sensitive compounds since they would hydroly#e as well.
FEATURES
$igital display for rotation speed, vapor temperature and bath temperature
%onvenient controls for ad&ustment of rotation speed and heating bath temperature
'otation speed from ( rpm to )* rpm
+iniature circuit breaker and separate power switches for control panel and heating
bath offers safety
,ne heating bath for water and oil- ambient to ()* .%
/ath temperature display accuracy 01- ( .%
$igital display for vapor temperature 01- ( .%
bath as standard
MUHAMMAD DANISH 1
31-02-07
ANALYTICAL TECHNIQUES
COURSE#509
APPLICATIONS
$istillation of solvents
%oncentration of solutions
%rystalli#ation
ynthesis 2 3urification
3owder 2 granules drying
ANATOMY OF A ROTOVAP
4 long condenser containing a distillation tube surrounded by a coil of glass tubing.
This glass tubing will have cold water running through it to provide a cooling
atmosphere for the gas as it is being distilled.
The condenser is hooked up to a vacuum line (either the house line or a pump). To
close the system, and thus activate the vacuum, turn the stopcock knob at the far end
of the rotovap. The system is now under reduced pressure.
4 large round collection flask is attached to the condenser to trap the solvent.
4 distillation tube connects the condenser to the sample flask. There is a 5bump flask6
at the end of the distillation tube to prevent unwanted sample from splashing up into
condenser. The distillation tube will carry the distilled solvent about halfway up into
the condenser before this gas will encounter the coils filled with cold water.
4 rotary dial is included that will allow you to spin the sample flask.
4 hot water bath is included that can be raised by turning the knob on the &ack below
the water bath clockwise. This is used to heat the sample flask.
%old water for the condenser coils is provided by a closed-loop water pump.
7hen using the vacuum pump, a liquid nitrogen trap is placed in the vacuum line
between the rotovap and the pump to prevent solvent vapors from attacking the pump
machinery.
USING THE ROTOEVAPORATOR
4dd your sample to be rotovapped into the roundbottom ('/) flask. The flask should
never be more than half full with liquid when you attach it to the rotovap. !f it is, you
risk losing some of your sample8 !f you have too much liquid to evaporate, remove
some until the flask is less than half full, rotovap away the liquid in the '/ and then
add the rest. ,r you can use a hot water bath in the fumehood to boil away some of
the excess solvent.
%onnect your '/ flask to the trap on the end of the distillation tube and secure this
using the circular clip. The clip has two sides9 the smaller circle goes &ust above the
lip of the '/ flask, on the neck of the trap and the larger circle goes &ust below the lip
of the '/ flask.
To close the system and activate the vacuum, turn the stopcock knob to close the
system and turn on the vacuum. The system is now under reduced pressure.
The liquid in the '/ flask can now boil at a lower temperature. "owever, you can
speed up the evaporation by rotating the flask, which throws more liquid on the walls
of the flask and increases the surface area for evaporation.
To speed up the rate of evaporation, the liquid sample can be warmed with hot water.
'aise the hot water bath until the hot water covers the liquid level in the '/ flask.
4s the solvent evaporates, its vapor will go through the bump flask into the distillation
tube and exit about halfway up the condenser coils. These coils are filled with cold
water and thus the hot gas will condense there. Very soon, you should notice liquid
dripping off the coils and collecting in the large condensate flask below the coils.
MUHAMMAD DANISH 2
31-02-07
ANALYTICAL TECHNIQUES
COURSE#509
7hen the dripping stops or you don:t notice any dripping off the coils for at least ;*
seconds, you can stop the rotovap. <ou do this in the reverse order from the way you
started9
=ower the hot water bath so that it is not touching the '/ flask and there is enough
clearance so that you will be able to safely remove the flask.
Turn the rotary dial to stop the spinning of the flask.
Turn off the vacuum.
,pen the system to atmospheric pressure with the stopcock.
'emove the >eck clip from the flask. !t is usually easier to do this if you turn the clip
to the back away from you, place your right hand around the '/ and your right thumb
on the nearest handle of the clip while grasping the opposite handle with your left
hand. 3ush back on the two handles and the clip should come off.
'emove the flask. 3lace your left hand on the bump flask and with your right hand,
slowly twist the neck of the '/ flask to break the vacuum. $, ?,T '@+,V@ the
flask by pulling straight downwardsA this can result in a loss of some of your sample in
the '/ flask. =eave your flask uncorked at this stage.
MODEL RANGE
There is a range of models covering an evaporation flask capacity from ( litre l to (** litres.
The ma&ority of these models may be used on the laboratory benchA the larger models ((*,
B*, C* 2 (** litres) are designed f
or use in pilot plants and production facilities.
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MUHAMMAD DANISH 3
31-02-07