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Using A Separating Funnel: Chemistry Department

1. Separating funnels are used to separate mixtures into aqueous and organic layers for solvent extractions in organic chemistry. 2. When using a separating funnel, make sure not to overfill it and keep the stopcock closed except when venting. Mix the layers thoroughly by inverting, opening the stopcock to release pressure, then closing and shaking until no more vapors are released. 3. Separate the layers into different flasks labeled for the aqueous or organic layer based on the relative densities of the solvents used. Repeat extractions to thoroughly separate the layers of interest into the desired flask.

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101 views

Using A Separating Funnel: Chemistry Department

1. Separating funnels are used to separate mixtures into aqueous and organic layers for solvent extractions in organic chemistry. 2. When using a separating funnel, make sure not to overfill it and keep the stopcock closed except when venting. Mix the layers thoroughly by inverting, opening the stopcock to release pressure, then closing and shaking until no more vapors are released. 3. Separate the layers into different flasks labeled for the aqueous or organic layer based on the relative densities of the solvents used. Repeat extractions to thoroughly separate the layers of interest into the desired flask.

Uploaded by

PaxChem Ltd.
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Using a separating

funnel

Chemistry Department
Separating funnels are used for carrying out solvent extractions in organic
chemistry. They can come in different shapes and volumes, make sure you
use a suitable volume for your extraction and never fill the separating
funnel more than two-thirds full.
When transferring liquids into the separating funnel you should make
sure that the stopcock is closed and that the funnel is adequately
supported, using a clamp or a ring.

When pouring liquids


into the separating
funnel you may wish
to use a measuring
cylinder or a long-
stemmed glass
funnel to minimise
any spillages
Separating the layers is usually the part most find difficult.
The main reason for this is not knowing which is the aqueous
and organic layers. The table below lists a number of
extraction solvents along with their relative densities:

Solvent Density (g/cm3)


Petroleum ether Typically ~ 0.640
Diethyl ether 0.714
Toluene 0.867
Ethyl acetate 0.900
Water 1.000
Dichloromethane 1.327
If your separation has gone well you should easily see two
visible layers in the separating funnel. Here we have added
colour to the aqueous and organic layers to show the
separation more clearly, but for your separations there
will be no colour.

Upper layer Upper layer


(Orange) (Red)

Lower layer Lower layer


(Red) (Orange)

NOTE: In both separating funnels, the red layer is the aqueous layer. But
how can this be?

Explanation: Look at the table on the previous slide. In the left separating
funnel, the aqueous layer is on the bottom, meaning the organic layer must
be less dense than water. In the right separating funnel, the aqueous layer
is on the top, meaning the organic layer must be more dense than water.
Video 1
Screen capture walkthrough, with
annotations
Note: CO2 is evolved
during extractions using
aqueous carbonate or
In order to carry out an efficient bicarbonate solutions!
extraction the organic and aqueous Be aware of pressure
build-up!
layers must be thoroughly mixed. Here
is a series of pictures that are screen
captures of an accompanying video.
Video 1: Screen shots
1. Insert the stopper 2. Remove the separating funnel from the
ring

Ensure solid grip


is used when
holding the
separating
funnel. One
option is to put
the stem
between your
forefinger and
middle finger

Stem of flask
Video 1: Screen shots
3. Place one hand around the stopcock and keep the other over the stopper at all times

Ensure the stopper is firmly in the


palm of your hand that you have a
good grip at the top of the flask

To reiterate, ensure solid grip is


used when holding the bottom of
the separating funnel.
Stem of flask
Video 1: Screen shots
4. Invert the funnel and immediately open
the stopcock to release any pressure
build up - when venting a funnel never
point the stem towards your neighbours
or yourself
Note: Whilst not shown
to the left (for ease of
demonstration), always
try and keep two hands
on the separating funnel. 5. Close the stopcock.
This is shown properly in Continued over
a few slides page

Tap open: allows venting

Always ensure you close


the tap before turning it
the right way round!
Video 1: Screen shots
5. Close the stopcock and gently shake the mixture, release the pressure again by
opening the stopcock
6. Repeat step 5 until no more vapour is expelled from the tap

Release pressure
by venting. Note
Close tap Gently shake the mixture tap is open.

Repeat until no more vapour is expelled


Video 1: Screen shots
7. Close the stopcock and return the separating funnel to the ring
8. Remove the stopper

Close tap Return to retort ring Remove stopper


(essential for
next step.
Video 2
Screen capture walkthrough, with
annotations.
Note: CO2 is evolved
during extractions using
aqueous carbonate or
Here is a series of pictures that are bicarbonate solutions!
screen captures of an accompanying Be aware of pressure
build-up!
video.

It is now time to separate the layers into two different conical flasks, one for
your aqueous layer and one for your organic layer (remember, colouring has
been added here for emphasise – both your layers are likely to be colourless.

Note: This extraction is generic. You will need to determine whether you
are extracting your aqueous layer with organic solvent, or vice versa. On
this occasion, the red layer (bottom) is being extracted by the orange layer
(top – called ‘extraction solvent’)
Video 2: Screen shots
1a. Separate your two layers into two different conical flasks
Remember: The layer being extracted does not necessarily have to be the bottom
layer. It could also be the top layer

Layer being extracted

Extraction solvent

Open tap to run out


bottom layer. Take
care to keep layers
separate.

Two different
flasks. Make sure
you label them
properly (your
solutions will be
colourless!)
Video 2: Screen shots
1b. Separate your two layers into two different conical flasks

Put empty flask under


separating funnel and
Close tap collect extraction solvent Nicely separated
Video 2: Screen shots
2. Return the layer being extracted (red 3. Add some more of your extraction
here) to the separating funnel solvent (orange), and repeat the
(perhaps use a long stemmed funnel shaking out process (see points 1-8 of
to minimise spillages) video 1)

Pour in ‘new’ extraction


Return the layer solvent from measuring Back to similar
being extracted cylinder situation as stage 1.

Note the
amount in
measuring
cylinder has
decreased
Video 2: Screen shots
4. After shaking and venting (steps 1-8 of previous video), separate your two layers
again, you can combine this portion of extraction solvent (orange) with the previous
extraction solvent (orange)

Remove layer being Combine this portion of


extracted into its extraction solvent with
Nicely separated
original flask previous portion
Video 2: Screen shots
5. Repeat steps 2, 3 and 4 once more
6. You now have your two separate
layers, make sure you know
which one you need for further
processing

Your extraction is finished. If the


organic layer is the layer of interest
(usually, but not exclusively), you
should move onto drying the organic
layer

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