A Beginners Guide to the Rotary Evaporator

Tom Aborn
Introduction
The goal of organic synthetic chemical research is to learn about the mechanisms
and products on new chemical reactions. Many chemical reactions, like the infamous
baking soda and vinegar volcano reaction, occur instantaneously. Organic reactions,
however, tend to be long, slow, arduous processes that take hours, days, and sometimes
even weeks to run to completion. To epedite the process, chemists use solvents in their
reactions. !or the purposes of this guide, a solvent will refer to the low boiling, non"
reactive li#uid that is used to dissolve the reagents $ingredients%. &olvents help to mi up
the reagents of the reaction and make sure they come into contact more fre#uently,
meaning that they will react more fre#uently, and thus speed up the overall process of the
reaction.
There is a draw back to using solvents, however. 'hen the reaction is finally
completed, the solvent will still be mied in with the product of your reaction, meaning
that your data concerning the product of your reaction will be corrupted by the solvent.
This isn(t too much of a problem for an undergraduate chemistry lab, because it is
possible when analy)ing your product to discern which data relates to the compound you
made, and which data refers to the solvent that was used. *n a professional
pharmaceutical lab, however, you cannot present a drug you have made for testing if it
still has solvent mied into it. 'hile solvents are great for moving chemical reactions
along, they are not to be ingested and can often be harmful to the body. Therefore, it is
necessary to find a way to completely remove the solvent from your product. One way of
doing this is to use the rotary evaporator $rotovap%.
How the Rotovap Works: A basic overview
Figure : !iagra" o# a typica$ rotary evaporator% &hoto courtesy o#
http:''www%#$ickr%co"'photos'danes()'*+,*-.*'%
The rotovap takes advantage of the low boiling points of solvents by creating an
environment where the solvent will rapidly boil off leaving only your product.
+onditions that are most conducive to boiling are, low air pressure and high temperature.
The -otovap works as such,
/A0 Round Botto"ed F$ask: This flask contains your product and the solvent you
are trying to remove. *t is attached to an ale that rotates the flask. This creates
a thin layer of solvent miture on the sides of the flask that will evaporate more
#uickly.
/B0 Heating !ish, The heating dish is filled with distilled water, which is heated and
begins the evaporation process.
/10 1ondenser 1oi$: As the solvent begins to evaporate, the glass case surrounding
the coil will begin to fill up with vapor. The condenser coil will help to condense
the vapor back into li#uid to avoid dangerous pressure buildups.
/!0 Water Hose: Attached to an eternal water source, the water hose runs cool
water through the condenser coil $.% and keeps it cool enough to allow the vapor
to condense on it.
/E0 2acuu" Hose: +onnected to an eternal vacuum pump, the vacuum hose
removes the air from the chamber surrounding the condenser coil $.%. The
removal of air pressure by the vacuum hose allows the solvent to evaporate faster
and with less heat re#uired from the heating dish $/%.
/F0 &ressure 2a$ve: +uts the chamber surrounding the condenser coil 0 off from
the atmosphere, preventing any air pressure from replacing the air removed by
the vacuum hose $1%.
/G0 1o$$ection F$ask, 'hen the evaporated solvent condenses on the condenser coil
$.%, it drips down into the collection flask. 'hat you do with the etra solvent is
up to you.
/H0 1ontro$ &ane$: This panel contains the controls for raising and lowering the
round bottomed flask in and out of the warm water in the heating dish $/%, the
controls for the speed of rotation of the flask, and controls for how warm the
water in the heating dish is.
Instructions #or 3sing the Rotovap:
2se the following steps to safely remove the solvent from your product.
1A34I56, A3'A4& use proper eye protection when in the laboratory.
% 5our your miture into a round bottomed flask. +hoose a flask big enough so that
it is no more than half full with your miture. *f necessary, use two flasks and
rotovap them separately.
.% Attach your round bottomed flask to the apparatus, using a clip to fasten it into
place.
+% Attach vacuum hose $1% to the top plug, and water hose $.% to the bottom plug.
-% +lose pressure valve $!% to prevent any air from entering the chamber.
7% 1nsure that your collection flask $6% is clasped firmly into place.
)% Turn on the vacuum and the water flow from their eternal sources. The water
pressure should be high enough that once it has flowed through the condenser
coil, the water is gently flowing from the eit hose $not shown%.
8% &ome rotovaps have a pressure gauge attached to read the pressure inside the
chamber. *f your rotovap contains a pressure gauge, wait until it reads around 788
torr or 8.79 atmospheres $atm%, based on what units of pressure the reader uses.
$:ote, Another unit that may be used is a 5ascal. A 5ascal $5a% is e#ual to ; torr.%
*% *f there is no pressure gauge, wait around ;8 seconds for the pressure to drop. *f
you have waited ;8 seconds or the gauge reads the proper pressure level, you are
ready to begin.
(% .O :OT turn off the vacuum or water hose, .O :OT open the pressure valve.
2se the control panel to heat the water bath to <8
o
+. *f your solvent does not
evaporate at <8
o
+ under the reduced air pressure provided by the rototvap, then
you need to find another way to remove your solvent.
,% Once the bath begins to heat, use the control panel to lower the flask into the bath.
*t should be lowered such that the flask barely touches the water, this ensures that
the miture is heated slowly. *f the miture is heated too fast, then your miture
will bump. &ee caution below.
% Once the flask is barely touching the water, use the control panel to begin rotating
your sample. The flask should rotate =ust enough that the solvent forms a thin,
filmy layer on the side of the flask. The rate of rotation re#uired is not high, but
may vary depending on flask si)e and the volume of your miture.
.% Allow your sample to rotate and heat for 9";8 minutes or more, depending on the
volume of your miture.
+% There is no definite way to know you are done. 'atch the volume of your
miture and the amount of solvent collected in the collection flask to make an
educated guess as to how much heating>rotation is necessary.
-% 'hen you think you are done, stop the rotation and raise the flask out of the
water.
7% T2-: O!! the vacuum hose.
)% Turn off the water hose.
8% O51: the pressure valve.
*% 'A*T 2:T*3 T?1 A*- 5-1&&2-1 ?A& /11: -1&OT-1. TO T?1
+?AM/1- /1!O-1 -1MO@*:6 4O2- M*AT2-1. &ee warning below. *f
your rotovap has an air pressure gauge, wait until the gauge reads around B<8 torr
$or 5A% or around ; atmosphere $atm%. *f you do not have a gauge, you can listen.
'hen you open the valve you should hear the air rushing into the chamber,
making a whistling"like sound. 'ait 9";8 second until A!T1- the whistling has
subsided to proceed.
(% 'hen the whistling has subsided and air pressure is restored to the chamber, you
may unclip your sample and remove it from the rotovap.
1A34I56: /umping is, in laymen(s terms, a hard bubble, the miture bubbles so
hard that it flies out of the flask all over the chamber. That is very bad and may ruin your
miture, do not let it happen.
WAR6I6G: *f you attempt to remove your flask from the rotovap /1!O-1 air
pressure has been restored to the chamber, your sample '*33 bump. *t will bump so
hard that your sample will fly out all over the chamber and be lost, and you will have to
start your eperiment all over. Trust me, * know.
3ast updated Thursday, April 8;, 78;8
-otary evaporators $also called CrotavapsC% are used to remove solvents from reaction
mitures and can accommodate volumes as large as D liters. They are found in almost
every organic laboratory, since they allow performing this task very #uickly. A typical
rotary evaporator has a water bath that can be heated in either a metal container or
crystalli)ation dish. This keeps the solvent from free)ing during the evaporation process.
The solvent is removed under vacuum, is trapped by a condenser and is collected for easy
reuse or disposal. Most labs use a simple water aspirator vacuum on their rotavaps, so a
rotavap cannot be used for air and water"sensitive materials unless special precautions are
taken i.e. additional traps are used. *n the lab, the house vacuum line, a circulation bath or
a membrane pump are used as source for the vacuum $<8"98 torr%. 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 $see table below%.
9o$vent b%p% /8), torr0 b%p% /-, torr0
acetonitrile E;.E
o
+ B.B
o
+
diethyl ether D<.F
o
+ "7B.B
o
+
ethanol BE.<
o
+ ;G
o
+
ethyl acetate BB.;
o
+ G.;
o
+
heane FE.B
o
+ "7.D
o
+
heptane GE.<
o
+ 77.D
o
+
methanol F<.B
o
+ 9.8
o
+
water ;88
o
+ D<.8
o
+
&ince the flask is rotated during the evaporation process, the surface area is larger than
normal which increases the evaporation rate significantly. The solvent is collected in a
flask and can properly be disposed off afterwards $organic solvent waste%. *n addition,
this method also avoids overheating of the target compound i.e. oidation because lower
temperatures are used. The same rules like for vacuum filtrations apply here in terms of
the glassware and other precautions i.e no cracks on the flask, etc.
Genera$ ru$es #or usage o# a rotary evaporator
6eneral rules for usage of rotary evaporators
;. The solvent collection flask of the unit should always be emptied prior use to prevent
accidentally miing of incompatible chemicals. &A!1T4 !*-&TH
7. The flask with the solution is placed on the rotary evaporator. The use of a bump trap
prevents the solution from accidentally splashing into the condenser $and being
contaminated%. *t is highly advisable to start with a clean bump bulb in case something
bumps over after allH This would allow the eperimenter to recover the solution or solid.
D. A metal or Ieck clip is used to secure the flask and the bump trap. The green one
shown below fits 7<><8 ground glass =oints. &imilar blue clips fit ;G>77 =oints and the
yellow ones fit ;<>78 =oints, which will most likely used in the lab. I# you break the
bu"p trap: you wi$$ have to pay #or it;
<. The dial on the motor is used for speed control of the flask rotation. A typical rotavap
uses a variable speed sparkless induction motor that spins at 8"778 rpm and provides high
constant tor#ue. A good setting here is B"E.
9. The aspirator vacuum is turned on. On most models, the vacuum on>off control is
managed by turning a stopcock at the top of the condenser $left side of the above
diagram%. This stopcock is later also used to vent the setup after the solvent is removed.
F. The flask is lowered into the water bath $or the water bath is raised to immerse the
flask in the warm water. $On most models, a convenient handle $with height locking
mechanism% moves the entire condenser>motor>flask assembly up and down. Often the tilt
of the condenser assembly can also be ad=usted. The water bath temperature should not
eceed the boiling point of the solventHH !or small amounts of common solvents the bath
heater is not needed.
B. The solvent should start collecting on the condenser and drip into the receiving flask.
&ome solvents $such as diethyl ether or dichloromethane% are so volatile that they will
also evaporate from the receiving flask and be discharged down the drain. To prevent
this, a cooling bath on the receiver or $on some models% use a dry"ice condenser can be
used. *n addition, an additional trap $with dry"ice or li#uid nitrogen% can be placed
between the vacuum source and the condenser unit. This is particularly important of a
membrane pump is used as vacuum source.
E. Once all the solvent evaporated $or whatever is desired at this point%, the vacuum is
released,. The flask is raised out of the water bath and the spinning is discontinued.
G. The bump trap has to be cleaned and the receiving flask is emptied upon completion of
the evaporation.
4ips and 4ricks
Tips and Tricks
.istilled water should be used in the heating bath to minimi)e the scale build up in the
bath which coats the thermistor and heating coils. *t is very difficult to remove and
reduces the efficiency of the bath. *n addition, regular tap water will promote the growth
of spectacularly disgusting algae colonies, particularly during the summer months. The
best protocol is a regular echange of the water.
To remove algae gunk from the inside of a coiled water condenser, the condenser has to
be removed from the rotavap and the coil is soaked in a dilute nitric acid solution for a
few hours. After carefully rinsing the insides, the rotavap is reassembled. All standard
safety precautions should be followed when working with nitric acidH
The ground glass =oint holding the flask does not need to be greased, but on rare
occasions it $or the bump bulb% may get Cfro)enC. &ome companies sell special =oint clips
that can free fro)en =oints simply by screwing them in one direction. *f you are not lucky
enough to have these and cannot release the =oint you probably want to ask your teaching
assistant for advice.
*f a mechanical pump is used instead of an aspirator to produce a vacuum, a secondary
trap has to be used to prevent that the solvent destroys the membrane or is absorbed in the
oil.