Carrying out a vacuum filtration

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Language: en

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Once you've done your recrystallisation and
you've got your hot filtrate this
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needs to be cooled to room temperature.
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If you want to do this quickly can use
an ice bath.
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However you will get best crystals if you
allow it to cool down slowly.
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If you do need to do this quickly, then use an
ice bath, immerse your flask in the ice.
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If you want to leave this for a while make
sure you clamp your flask.
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You can see the crystals are already coming out of solution.
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Make sure you allow the filtrate to cool
to room temperature or below the
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crystals can then be collected by
filtration.
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It's a good idea, however to keep the
filtrate just in case you don't get a
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good yield.
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We're going to use a Buchner funnel to
collect the crystals.
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Turn the water aspirator on full and
connect it to the flask, so we apply
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reduced pressure to the flask. Make sure
the funnel is well sealed.
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You can use a few drops of the solvent to
seal the filter paper.
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Then carefully pour a small amount at a
time with the filtrate containing the
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crystals into the middle of the filter
paper.
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You can use some of the cold solvent to
rinse the flask.
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Swirl it around to try to get the
remainder of the solid out.
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You can now use a small amount of the
cold solvent to rinse the crystals don't
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use too much though as you will start to
dissolve them. Take the tubing off the flask
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before you turn the tap off. Otherwise
you will get water sucked back into the flask.
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If you have got less material you could use a Hirsch funnel instead which works in the same
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principles as a Buchner funnel.
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You've got a filter paper covering the
holes in the bottom of the funnel
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and a side arm which is attached to the water
aspirator.
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Obviously the volume for the filtrate is
a lot small as you need to make sure
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you're not filtering too much.
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Once you have separated your products
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it's a good idea, if you have time, to dry
it in a vacuum desiccator.
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Carefully remove the filter paper from the Buchner
funnel.
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Place it onto a bigger piece of filter
paper and sandwich it between another piece.
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Then turn the edges over to make a parcel.
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It's a good idea to do this because when
you come to open the vacuum desiccator
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after drying the crystals. They can
easily be disturbed by the air flow
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through the tap whilst the pressures are
equalising. This is a vacuum desiccator,
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if you take the outside cover off you'll
see that there is a drying agent in the
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base, covered by a metal gauze, which is
where we're going to put our compound.
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You can use a variety of drying agents
but this is anhydrous calcium chloride.
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We're going to put our compound on top
of the gauze and put the lid on. What
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we're going to do here is create a very
dry atmosphere using this drying agent
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under reduce pressure because we're
going to do this under reduce pressure
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we need to put a cover over the
desiccator.
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Turn the aspirator on,
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make sure the tap is open and attach the
tubing. Leave this for five minutes or
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so, close the tap,
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remove the tubing and turn the water tap
off.
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When you come to open the desiccator,
make sure you open the tap slowly so the
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flow of air back into the desiccator is
slow.
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Once the pressure is equalised take the
cover off,
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Remove the lid, and take the crystals out.
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The crystals should now be dry and ready to have a melting point taken,
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or further characterisation
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