Video Transcript
In this video, we will learn how to
separate mixtures using filtration and crystallization. We will also learn how to decide
which apparatus we need and which method should be used.
In experimental chemistry, being
able to purify and separate different substances is a key skill. Two useful methods in this area are
filtration and crystallization. Let’s look more closely at what
each of these methods can achieve.
Filtration, for example, is useful
for separating a solid from a liquid. A good example where we use
filtration in everyday life could be how to get coffee grounds from a cup of
coffee. On the other hand, crystallization
is useful for getting a solid out of solution. An example of this which you may
have come across is getting copper sulfate crystals from a copper sulfate
solution. While at first glance it may seem
like actually these two are doing the same thing, i.e., getting a solid and liquid
to come apart, there are actually some key differences. For example, in filtration, the
solid which we are separating is insoluble in the liquid we are separating it from,
just like coffee grounds and water. However, in crystallization, we
have a solid which is soluble in the liquid which we are trying to separate it
from. And this is an important
difference.
Let’s begin by taking a closer look
at how we carry out filtration. When it comes to filtration, there
are two main methods. These are gravity filtration and
vacuum filtration. Gravity filtration is quite a lot
slower than vacuum filtration. However, gravity filtration tends
to be better than vacuum when it’s the liquid which is the part that you want to
keep. Moreover, gravity filtration is
good when you have a large volume of liquid which you need to filter. Vacuum filtration is faster than
gravity filtration, and it’s also better for filtering small amounts of solid or
filtering small amounts of liquid. It’s not as good as gravity
filtration if you have a lot of solid or a lot of liquid to get through. Don’t forget that you can also
perform gravity filtration as a hot filtration. This is useful if while filtering
you get crystallization occurring inside the filter funnel.
So let’s have a look at how gravity
filtration works. In order to carry out gravity
filtration, you’re going to need an Erlenmeyer, sometimes called a conical, flask
and a funnel. In order to make sure that nothing
gets knocked over, you should secure your funnel with a clamp or a ring stand. Notice that the conical or
Erlenmeyer flask doesn’t need clamping because the positioning of the funnel will
hold it securely. When you need to remove the
Erlenmeyer flask, you simply loosen the clamp on the stand and slide the funnel up
the pole. This then gives you the space to
take out or put in a conical or Erlenmeyer flask. Don’t forget that your clamped
glassware should always overhang the heavy base on the retort stand. This prevents anything from
toppling over.
The last piece of equipment we’re
going to need is a filter paper. Filter papers are circular and come
in lots of different sizes. They’re very much like the same
filters you’d use to make filtered coffee. In order to get this circular
filter paper inside our funnel, we need to fold it. We could fold it into quarters,
which would then give us a cone. However, using this method, there
would be a part of our cone which has a double layer of filter paper. Having two layers of filter paper
for our solution to get through is going to make our filtration even slower. And remember that gravity
filtration is slower than vacuum filtration already. So, while we could use this method,
it’s not the most effective. Instead, what we do is we flute the
filter paper. This means folding it into lots of
small triangles and then alternating which direction these go so it concertinas
up. While this can be more fiddly to
do, it means that when we filter whatever it is, it only has to go through one layer
of filter paper regardless of where it is. With practice, this will become
much easier. Once we fluted our filter paper, we
can sit it inside our funnel and begin our filtration. So, our first step is always to set
up our apparatus.
The next thing we’ll want to do is
to swirl the mixture that we’re going to filter. This means that any particulates at
the bottom of our mixture can be thoroughly mixed throughout the liquid. This is especially important if
it’s the particulate matter that we want to collect. If you don’t swirl it, some of that
matter might remain in the conical or Erlenmeyer flask and not pass through your
filter paper. This then makes it a tricky job to
get out of the flask.
Next, we can pour our swirled
mixture into our fluted filter paper. You should do this slowly and
gradually, swirling again if needed. Be careful not to overfill the
funnel. You don’t want any of that mixture
creeping over the edge of your filter paper and passing down into the flask. This would mean that some of your
solid isn’t caught, and you’d have to do this all over again. If it gets full, let it drain and
then add a bit more. What should happen is that the
solid particles will remain on the filter paper and your liquid will continue
through into the flask. This means we have successfully
separated a solid from a liquid. So if this is how gravity
filtration works, how is it different in vacuum filtration?
Let’s begin looking at vacuum
filtration by setting up our apparatus. We’re going to need a flask which
looks a little bit like an Erlenmeyer flask but it has a glass arm attached. This arm is where we can attach a
tube to our vacuum line. Remember that vacuum tubing should
be thick walled, not to be confused with the thin-walled tubing you would use for
water or gas.
The next piece of apparatus we’ll
need is a vacuum seal. This is usually a round rubber ring
which sits on the top of our flask and will hold our funnel in place. It helps to create a seal all the
way around. Next, we’ll need our funnel. But this is not a glass
conical-shaped funnel like we used in the gravity filtration. This one is more cylindrical and
usually made of ceramic. If you look at the funnel from the
top down, you’ll see that it has lots of small holes in the ceramic bottom. This type of funnel is called a
Büchner funnel. And the flask with the side on
which we are using is called a Büchner flask.
Just like with gravity filtration,
our apparatus should be attached to a stand to keep it secure. This time, we’ll secure it to the
retort stand with a clamp around the neck of the Büchner flask. Be careful not to overtighten this
as you don’t want to damage the glass of the flask. It’s important to make sure all of
this is secure before applying your vacuum. If it’s not secure and you turn on
the vacuum, it could pull everything over.
Next, we’re going to need a filter
paper. When you put the filter paper
inside your Büchner funnel, it should cover all the holes. If any of the holes are showing,
the filter paper you’ve chosen is too small. So, you should change it for a
larger one. Equally, if your filter paper is
too large, it will crinkle and fold. This means that you could get some
of your mixture slipping down through the funnel without going through the
paper. This means some of the solid could
escape through, and you’ll have to do this all over again. Make sure that you pick the filter
paper which is just the right size.
Once our apparatus is all set up,
we can begin filtering. First, we can turn on the vacuum to
our Büchner flask. Next, before we actually begin
filtering, we need to test our vacuum seal. To do this, wet your filter paper
with just a small amount of solvent. Try to choose the same solvent
that’s going to be in your mixture that you’re going to filter. So, if you’re filtering sand out of
water, you should use water to wet your paper. If you’re filtering some kind of
solid out of ethanol, you should use ethanol to wet your paper.
Once the paper is wet, if the
vacuum seal is good, you should hear a sucking noise. Equally, if you gently try to move
your Büchner funnel, you should feel that it’s gripped tightly by the vacuum. This means you have a good
seal. If you don’t have a good seal, now
is the time to try to solve the problem. It could be you just need to jiggle
the funnel around in the vacuum seal, or maybe your seal is damaged and you need to
replace it. Either way, it’s important to get a
good seal before starting to filter.
Just like in gravity filtration,
you should swirl your mixture to make sure that you have a good mix of the
particulates and they’re not all stuck to the bottom of your vessel. You can then gently and slowly pour
this mixture into your Büchner funnel. The vacuum should quickly suck the
liquid through into the flask with a satisfying bubbling and gurgling. Any solid particulates should be
left on the filter paper in your Büchner funnel. If at any point your filter paper
starts to wrinkle or come away, stop pouring. Make sure that your filter paper
stays flat at all times. This stops any solid slipping
through into your flask.
If your filter paper gets covered
in a thick layer of solid, it can decrease the amount of vacuum you have and block
the paper up. To fix this, you may have to pause
your filtration. You could gently try to move some
of the solid, but that risks tearing the filter paper. So, if you do try that method, you
must be very careful. If there’s no liquid in your
Büchner funnel, it might be easier just to change your soiled filter paper for a new
one.
You also need to keep an eye on the
level of the liquid in your Büchner flask. If your Büchner flask gets quite
full, it needs to be changed out. If the liquid reaches the height of
the glass arm, you’re going to suck liquid into your vacuum line, which is really
bad. This is why vacuum filtration is
best for filtering mixtures which only have a small amount of solid or a small
amount of liquid.
Now that we’ve separated insoluble
solids from liquids, let’s look at separating soluble solids from liquids. To achieve this, we use
crystallization. To carry out crystallization, we’re
going to need an evaporating basin, which is held over a heat source, for example, a
Bunsen burner. We place our solution inside the
evaporating basin and turn on the heat.
As we begin heating our solution,
the solvent begins to evaporate off. As we evaporate more and more
solvent, think about what happens to the concentration of our original solution. With less solvent, our solution
becomes more and more saturated, until it’s supersaturated. If we were to then turn off the
heat, our solution would cool down, and you would notice that crystals would start
to form. This is because as our solution
cools down, it’s not able to hold quite so much solid in solution. This excess solid falls out as
crystals.
We could then use one of our
filtration methods to filter off our solution that remains and keep our lovely new
crystals. And this is certainly one method
for carrying out crystallization. This method means that if there are
any impurities in our solution, they don’t also come out as crystals. So you can consider this a
purification step, but it’s not the only method of crystallization.
Another method to obtain crystals
from our solution is to simply keep heating it. As we get rid of more and more
solvent, less of the solid can remain in solution. So you’ll notice that some solid
forms on the edges of the evaporating basin. We simply need to keep heating
until all of our solvent is gone, leaving behind all of our solid as crystals. The downside to this method of
crystallization is that if there were any impurities in your original solution,
these will also have come out as crystals, contaminating your lovely solid
sample. So a further purification step
would be required. This method also produces much
smaller crystals than if you only evaporate the majority and then leave it to
cool. If you have the time and patience,
you can get some really lovely large, regular crystals from the first method. You may have done this with copper
sulfate solution, for example.
Let’s summarize what we’ve learnt
about filtration and crystallization. Filtration can be used to separate
insoluble solids from liquids, for example, sand from water. We can use gravity filtration,
which is slow but good for large volumes. This involves an Erlenmeyer flask,
funnel, and fluted filter paper. Or we could use vacuum filtration,
which is quicker but not so good for large volumes or large amounts of solid. Vacuum filtration involves a
Büchner flask, Büchner funnel, and vacuum line.
On the other hand, crystallization
is good for separating soluble solids from their solution, for example, getting
copper sulfate crystals from copper sulfate solution or perhaps getting salt
crystals from salt water. This technique involves evaporating
solvent from your solution to supersaturate it. You can either then cool it to
produce large crystals or continue evaporating all of your solvent to create smaller
crystals.