Experimental Techniques

Measurement
CIE wants you to demonstrate the ability to
name the appropriate apparatus for the
following: Time, temperature, mass,
volume:
1. Time
 Digital stop watch
 Measures up to 0.01s
2. Temperature
1. Mercury-in-glass thermometer
 Measures up to nearest °C
3. Mass
0. Electric top-pan balance
 Measures up to 0.01g
4. Volume
0. Beaker
 Used to estimate liquid volume
1. Measuring cylinder
 Measures up to 0.1cm3 (More
accurate than beaker)
2. Pipette
 Measures fixed volumes of liquids
accurately (i.e. 20cm3)
 Measures up to 0.1cm3
3. Burette
  Used for measuring variable
volumes of liquids accurately
 Measures up to 0.1cm3
Criteria of purity
The purity of a substance is defined as the
degree to which a substance is undiluted or
unmixed with other material. A pure
substance therefore would be made of
a single substance.
Purity assessment from melting
point/boiling points
The melting point of a substance is the
temperature in which the substance melts.
Similarly, the boiling point of a substance is
the temperature at which it boils.
Interestingly, the boiling point and melting
point of a substance can give us an
indication of how pure it is. The table below
summarizes this quite well (Hodder IGCSE
Chemistry Revision Guide):

Paper chromatography
Paper chromatography is a separation
technique that is used
to separate and identify the components in
a mixture.
How it works is fairly easy. Lets imagine you
have an unknown liquid (Liquid A). You
want to find out whether or not this liquid is
impure (i.e. a mixture) and if so, how many
substances are in this mixture and what
exactly are they?
Firstly, you simply get a drop of liquid A and
place it onto the chromatography paper.
You then draw a horizontal line marking
that drop (you’ll see why this is important
later).
You then set up the chromatography paper
inside a beaker so that the bottom of the
paper is just immersed inside the solvent
(propanone or water). An example of this
set up may look like this:

As time passes, the solvent will

travel up the chromatography paper. As the
solvent moves up, the sample spot of liquid
A will dissolve in the solvent. If liquid A was
a mixture, the various substances inside the
mixture will begin to separate because they
have different solubilities. Some substances
will travel up the paper slower than others
and reach a different end point. The end
result may look like this:

In this particular example, it is clear that the

ink spot (liquid A) is a mixture. Why?
Because you can see that it has separated
out into 3 different components (green,
purple, and yellow. If liquid A was pure then
you would only see one component.
*If liquid A was colourless, then the process
can be carried out exactly as before but a
locating agent will be required to “locate”
all the separated spots later in order to
measure the Rf values
Finally, since we know that liquid A is a
mixture, we can actually determine what
each of the substances are exactly. To do
so, we need to calculate the Rf value of
each of the separated components on the
chromatogram.
Rf Value = Distance traveled by spot /
Distance traveled by solvent
So lets go back to the example above:

The Rf value for:

 Green spot: 5 / 6 = 0.83
 Purple spot = 3/6 = 0.50
 Yellow spot = 1/6 = 0.17
All substances have a unique Rf value, and
therefore you will be able to find out what
exactly the substance is if you have a
reference table. In an examination, they will
always provide you with this.

Methods of purification
Filtration, centrifuging, decanting
All of these these methods are used to
separate an insoluble solid from a liquid.
 Filtration is carried out by pouring the
mixture into a funnel covered by a filter
paper. Whilst the liquid will pass
through the filter, solids will get caught,
thereby separating them.
 Centrifuging is a technique which uses a
spinning tube. The spinning generates a
strong centripetal force which causes
denser materials (i.e. solids) to travel
 towards the bottom of the centrifuge
tube at a faster rate than normal gravity.
 Decanting is the simple process of
letting insoluble solids settle in the
liquid before gently pouring it out later.
Evaporation
This is a simple process of separating the
crystals of a solute from a solution. Simply
let the solvent evaporate off and it will
leave the solids behind.
Crystallization
This technique is used to separate two
soluble solids from a solution (given that
they have different solubilities). It works by
dissolving the two solids in minimal water,
and then slowly cooling it. The less soluble
salt will crystallize first.
Simple distillation
This method is used to separate a
volatile liquid (easy to evaporate) from a
solution with a non-volatile solid. For
example, salt water can be purified using
this method. The equipment set-up is as
follows:
The heat causes the water to vaporize,
leaving the salt behind. The water vapor
then turns back into (pure) water as it
passes through the condenser (which cools
the vapor down).
Fractional distillation
This method is used to separate the
different liquids from a liquid mixture. For
example, a mixture of water and ethanol
can be separated using this method.
Fractional distillation works by using the
fact that different liquids have different
boiling points. It is a bit more complicated
than simple distillation but here is how it
works:

For arguments sake, lets say the round flask

contains a mixture of liquid A (boiling point
50°C) and liquid B (boiling point 100°C).
As you heat the flask with the Bunsen
burner, the temperature of the
flask and the fractionating column will
begin to rise. It is really important to
understand here that the bottom of the
long column is always going to be hotter
than the top. This is simply because we are
heating from the bottom and it takes time
for the heat to rise up.
So lets imagine the round flask hits 50°C.
What do you think will happen? Well, liquid
A will start to boil in the flask but the
vapour won’t get far in the column before
cooling back down into liquid (back into the
flask). This is because of the temperature
gradient in the column.
The very bottom of the column might
be 50°C but the top will be cooler than that,
meaning the gas will just condense back to
a liquid before reaching the top. Therefore
the main point to take away here is that the
gas can only go up as far as the
temperature in the column allows it to.
Eventually however, the column will heat
up sufficiently. When the top of the column
reaches 50°C, the vapour of liquid A will
reach all the way to the top and get
condensed into liquid by the condenser.
Once all of liquid A has entered the flask,
we simply need to replace it with an empty
one.
The column will then continue to heat up.
Eventually, the top of the column will hit
100°C whereby liquid B will reach the top of
the column and become liquefied by the
condenser and into our empty flask.
By utilizing the differing boiling points of
liquid A and B, we have successfully
separated it from the original mixture.

Purification summary
This is a handy summary from Hodder
IGCSE Chemistry revision guide:
NOTES OF
CHAP
EXPRIMENTAL
TECHNIQUES