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MIXTURE SEPARATION METHODS

In nature, the vast majority of substances are found in mixtures of many different types. In
many cases we make use of the substances that are part of a mixture. For example:

• We take the active ingredient of a medicine, which is mixed with other

ingredients and the excipient;
• At home we use cleaners whose antiseptics are mixed with detergents and water
as a vehicle.

However, in many cases it is necessary, or simply desirable, to obtain separately the

substances that make up a mixture, or to know the composition of such a mixture. This is
what chemical analysis is all about.
The components of a mixture can be concentrated or separated from the same me-
diante processes of separation.

A separation process is that which is carried out when a mixture them.

Filtration

It is the simplest of the separation methods. It is used whenever a solid is to be separated

from a liquid. What in a chemistry lab is called a filter, in cooking is called a strainer; if in
the kitchen we use a strainer or a sieve, in the lab we use a funnel with filter paper.

Distillation

It consists of bringing a liquid mixture to a boil in a distillation flask. The mixture can be
composed only of miscible liquids (which dissolve completely into each other) or it can
also contain some dissolved solids. Each of the liquids in the mixture retains its tendency
to evaporate and boil when it reaches near boiling temperature. The vapour that is initially
released is mainly composed of the liquid with the lowest boiling temperature (L1). This
vapour is passed through a refrigerant or condenser, and is collected in a container (see
Figure 1.12
Funnel with filter paper.
figure 1.13). While the temperature remains more or less constant, the vapour is composed
almost exclusively of L1. As all of the L1 has evaporated, the temperature rises to a point
where it reaches a constant level.
 CHAPTER 1 M a t t e r in n a t u r e 2 5

The boiling temperature of the next liquid, L2, which may be collected in another container,
is determined and so on. The solids in the mixture remain in the flask.

YOU FIND OUT:4

Alcohol content in some drinks
Watch the temperature of the steam generated, and
What percentage of alcohol is present in alcoholic make sure you only collect the liquid that boils at 78.5°C
beverages? (lower if you are not at sea level).
For each of the drinks, measure in a test tube
The main components found in these drinks are alcohol the volume of ethanol obtained from distillation and
and water. These two liquids have different boiling lime the percentage by volume of alcohol contained in
points: at sea level, alcohol (ethanol) is 78.5°C and each.
water is 100°C. This allows the distillation method to be Save the ethanol for future use.
used to stop the alcohol in each of the mixtures in a
fairly simple way, as it boils before the water. To carry
out a distillation, an equipment similar to that shown in With this information, he makes the calculations
figure 1.13 is needed. needed to answer the initial question.

Material
• Beer, brandy, rum
• Ball flask with "t" for distillation
• Glass thermometer
• Coolant with hoses
• 2 universal supports
• 2 three-finger tweezers with nut
• Lighter
• 1 iron ring
• Asbestos wire cloth
• Collection tube

Procedure
Choose a drink and place 30 mL in the ball flask. Start Figure 1.13
the distillation. Chemical laboratory distillation
equipment.

Crystallization

This process is mainly used when a dissolved solid (solu- tion) is to be separated into a
solvent. The solubility of a solute in a solvent generally has a limit, which is measured in
units of mass of solute per units of mass or volume of di- solvent at a given temperature.
This limit is known as saturation and we say that a solution is saturated if it does not
accept the solubilization of more solute. For example, it is known that the solubility of
sodium chloride (NaCl) is 39.12 g in 100 g of

4
The section "DISCOVER IT YOURSELF" is an invitation to carry out experimental work by proposing an
initiating question to which you must respond. The answer is not included, to be the product of practical enquiry.
Occasionally, the materials or procedures may be modified by you, with the help of your teacher, in case you
do not have exactly those mentioned in the work.
24FIRST TIME: Manifestations of matter
water, at 25ºC. If the volume of solvent decreases while the temperature remains constant,
the solute will tend to crystallize. As the solubility of a solute generally increases with
temperature, a decrease in temperature also favours crystallization of the solute.
It is possible that if two or more solutes are present in a solution, when partially
evaporating the solvent, only one of them will crystallize, the less soluble one. This can be
separated by filtration, and then continue to evaporate the solvent until the crystallization
of a second solute, and so on. This repetitive process, in which solutes of a solution are
separated from each other due to their different solubilities, is called fractionated
crystallisation.
Figure 1.14
Crystals under the
microscope.

DISCOVER IT YOURSELF:
Fractionated crystallization
(If you notice that a very small amount of undissolved
Which is more soluble in water, sugar or salt? crystals or some impurity remains, pass the mixture
through a brown filter paper).
You know, from experience, that both substances are Now place this solution in a glass cup (be careful
quite soluble in water, but to know the answer to the not to let the heat break the glass) and cover it, to keep
question, we suggest you carry out the following it free of dust. Leave it to rest for several days in the
experiment, which can be done even in the kitchen of refrigerator, during which time you will be able to
your house. observe the gradual appearance of crystals.
After a few days, when the increase in the amount
Material
of crystals formed is no longer noticeable, separate the
• Sugar
crystals by filtering the mixture with a coffee filter. In
• Go out
this case, and only in this case where the problem
• Measuring cup
substances are known and harmless, use your senses to
• Warming well
identify the nature of the crystals.
• Cooker
• Coffee filters
• Glass cups Can you now answer the question? Do you want to
• Refrigerator experience more?

Procedure
Dissolve 1/4cup sugar and 1/4cup salt in a cup of water.
Heat and stir until you reach the diso-

Figure 1.15
Separating funnel.
 CHAPTER 1 M a t t e r in n a t u r e 2 5

Extraction adding chloroform to this watery solution and shaking, S2 will remain in the water, while
S1 will be at least partially extracted by the Clo- roform. This procedure is carried out in
Water is not a separation funnel, as shown in figure 1.15. How much S2 remains in the water and how
miscible in much passes into the chlorine.
some liquids,
such as oil, or
in some
organic
solvents, such
as chloroform.
Whenever
these liquids
are stirred with
the intention
of mixing
them, they
separate again
into two
phases when
they are left to
stand. This
phenomenon,
together with
the greater or
lesser
solubility in
water of
certain types
of solutes
compared to
their solution
in other non-
water-miscible
organic
solvents,
forms the basis
of a separation
method known
as extraction.
Suppose
we have an
aqueous
solution in
which two so-
lutos are
dissolved, one
of which, S1,
is soluble in
chloroform (or
some other
non-water-
miscible
solvent) and
the other, S2,
is not. By
26FIRST TIME: Manifestations of matter

The amount of the dissolution depends on the particular affinity that S2 has for each of
these two solvents. In general, it is necessary to repeat the process several times, separating
the two phases and adding pure chloroform again to the aqueous solution.

DISCOVER IT YOURSELF:
Caffeine in a cola drink
With the collaboration of Rosa María González Muradas. Material:
• Separating funnel
Is there caffeine in Coca-Cola®? • Chloroform
• Coca-cola and/or prepared coffee
Caffeine is an organic substance whose condensed • Porcelain capsule
formula is: C8H10N4O2 and whose developed formula • Heating grid
is that of figure 1.16. • Extraction hood
This substance is
water-soluble. However... Procedure

The most important of CaffeineC8,H10,N4,O2

Place 50 mL of Coca-Cola in a separating funnel and
these is the affinity for add 50 mL of chloroform. Shake ten times, opening the
CH3
some organic solvents, funnel tap after each shake (to release the pressure
such as chloroform, N generated by the shaking). Let it rest until there is a good
CHCl3, which is almost NCH separation of
immiscible in

water. It is also known to N CH the two phases. Pour the clo-roma containing the
form needle-shaped N 3 extracted caffeine into a porcelain capsule.
crystals and to have a O Distil the chloroform from the solution into the
melting point of 238°C. CH3 water bath (save the distillate for another experiment)
until the dissolved solid is dry in the
It is then possible, by Figure 1.16 flask. In any case, it evaporates to dryness on a grill,
means of an extraction, Developed caffeine inside an extraction hood (the chloroform va- pores are
to separate the caffeine formula. toxic).
from an aqueous solution,

such as a Coca-Cola or a coffee, using chloroform. Identify the solid residue obtained. How would you
When the solvent evaporates, a solid is obtained that you know it is caffeine?
can identify by its crystalline form and melting point.
You can perform the experiment with prepared coffee and
compare the solids extracted in both cases.

Chromatography

This is one of the separation techniques that has evolved the most with modern technology.
The principles of chromatography are used to separate solids from solids (in solution),
liquids from liquids and gases from gases. The fundamental idea of chromatography is that
the components of the mixture to be separated are distributed between two phases, one of
which is fixed or stationary and the other, the mobile phase, moves through the first. This
passage of the mobile phase through the stationary one is known as the elution process.
The root chromos (colour) in the word chromatography has purely historical reasons.
It seems to suggest that colour is what distinguishes the components of the mixture, and
what makes them separable, but colour has nothing to do with it.
 CHAPTER 1 M a t t e r in n a t u r e 2 5

The first detailed description of a chromatography is attributed to Michael Tswett, a

Russian biochemist, who isolated chlorophyll from a mixture of plant pigments, in
28FIRST TIME: Manifestations of matter
1906. He placed a small sample on top of a column packed with
calcium carbonate powder and taught the sample with
petroleum ether (see Figure 1.17). As the sample descended the
column, it was separated into different bands that moved at
different speeds. The bands had different colours, due to the
nature of the pigments in the mixture, hence the name given to
Figure 1.17 the process, even though the colours were accidental and had
Chromatographic column.
nothing to do with the principle of the method.
According to the elution of
the mixture, several
containers are placed to
receive its different
components.

DISCOVER IT YOURSELF:
Dyes in gelatine
With the collaboration of Rosa María González Material:
Muradas • Strongly coloured gelatine powder (grapes, fruit,
etc.)
How many dyes can you identify in a powder for • Pasteur pipette
preparing gelatine? • Cotton
• Silica gel (for column chromatography)
The dyes used in foods are shaped by rather complex • Ethyl alcohol
organic molecules. The differences in the colours of • Sodium chloride
different substances are caused by differences in the
molecular structure that also make their solubility Procedure:
slightly different. It is these differences that allow us to Place a small cotton swab at the bottom of a Pasteur
apply the method of column chromatography to pipette (be careful not to get it into the capillary). Fill it
separate a mixture of such substances. You will carry with silica gel up to the upper third of the pipette and
out the se- paration in a microcolumn. insert another cotton ball.
Dissolve some flavoured gelatine powder in an
alcohol-water mixture in equal volume proportions and
shake to dissolve.
Add two drops of the above solution into the
microcolumn.
Add 5 mL of sodium chloride solution to
Figure 1.18 1%.
Microcolumn of this
experiment.
How many different dyes do you manage to identify?
 CHAPTER 1 M a t t e r in n a t u r e 2 5

Chemistry book consultation other type of procedure-- Electrophoresis

The separation of the two is different from that stated. A- Electrostatic precipitation
Here are some ideas:2. Investigate how they are carried out in the in-
Centrifugación It is used for filtering, distilling and
isotópica Extraction separation. isotópica Cite examples of
application in some
Distillation by dragging of specific vapor industrial process.