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() Subtopic 2.2

Purity
2.2 ()  Students taking questions in 24/24
this subtopic (by class):
2.2.0 ()

2.2.1 ()
Contents
2.2.2 ()
2.2.0 The big picture ()

2.2.3 () 2.2.1 Criteria of purity ()


2.2.2 Methods of purification ()
2.2.3 Checklist ()

Section 2.2.0

The big picture


 Students who have completed 23/24
this section (by class):

A pure substance contains only one type of particle (atom or molecule). As


a result, the particles within this substance are found in a very particular
arrangement. Impure substances contain more than one type of particle.
Impurities result in the original arrangement of the particles being
disrupted and consequently alters the boiling point and melting point of a
substance.

Chromatography can be used to separate and identify substances from


within an impure solution. There are several different types of
chromatography and its use within science ranges from identifying a
 particular mixture of ink found at a crime scene to identifying the likely
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(/) presence of a gene in a genetic test.  Help

During chromatography, substances move according to their mass and


()
solubility. Substances are separated accordingly and can then be identified
by comparison with previously known standards.
2.2 ()

2.2.0 () Watch this time-lapse video showing ink chromatography. See how the
colours are separated as they spread out.
2.2.1 ()

2.2.2 ()

Separation of Photosynthetic Pigments by Paper Chromatography


2.2.3 ()

Pure substances are obtained through several methods


including crystallisation, distillation and filtration, and through the addition
of a solvent. The method used to obtain a sample of pure substance varies
according to the challenge faced by the scientist.

Section 2.2.1

Criteria of purity
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Criteria of purity
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 Students who have completed 23/24


 () this section (by class):

2.2 ()

2.2.0 ()
Criteria of purity
2.2.1 ()

2.2.2 ()
Paper chromatography
2.2.3 ()
Paper
chromatography
can be used to separate and subsequently identify
small quantities of unknown substances within a solution. In biology, for
example, paper chromatography is commonly used to identify the
composition of mixtures such as the individual chlorophyll pigments found
within a leaf.

During paper chromatography, the unknown substances (


solutes
) are
carried up a sheet of filter paper by a
solvent
. The solutes move at
different rates according to their mass and solubility. They spread out and
are deposited (partitioned) at particular positions along the filter paper.

Each substance has a unique


Rf value
that can be calculated by dividing the
distance moved by the substance by the overall distance moved by the
solvent (distance from reference line to solvent front). Assuming that the
R
f
value of a pure substance (thought to be within the original mixture) has
previously been established and recorded, the
R
f
values of each unknown
solute can be calculated and the substance identified by comparison.

An overview of the paper chromatography process used to separate


unknown solutes from within a mixture by paper chromatography is shown

Figure 1
.
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g
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()

2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 ()

2.2.3 ()

Figure 1
. A diagrammatic overview of paper chromatography.

When the chromatography procedure has finished, the filter paper (with
solute spread out across the paper) is called a
chromatogram
. By simply
comparing the distance travelled by the unknown solute with the distance
travelled by the known comparator, you can tell if the unknown solute is
contained in the mixture.

The chromatogram in
Figure 1
shows that the unknown substance A is
composed of substance K, because substance K has risen up to the same
height as a substance in substance A. Substances B and C are still
unknown.


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The chromatogram produced from the separation of coloured inks shows


()
how simple inspection of the chromatogram can be used to conclude that
black ink is composed of red, purple, blue and brown inks (
Figure 2
).
2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 ()

2.2.3 ()

Figure 2
. The separation of coloured ink constituents using paper
chromatography.

Credit: Science Photo Library/IBL

 Practical

Aim

To separate ink pigments using paper chromatography.



S f t
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Safety
(/)  Help

A full risk assessment must be carried out before starting this


() practical activity (see
section 0.0.0
(/schoolstaff/app/cambridge-
igcse-chemistry-
2019/book/introduction/introduction/introduction/)
for more
2.2 ()
information). 
2.2.0 ()
Summary of method
2.2.1 ()
1. Place (using a pipette) a small volume of solute on a
2.2.2 () reference line approximately 1 cm from the bottom edge of
the filter paper. If more than one solute is to be tested then
2.2.3 ()
multiple spots can be placed on the reference line spaced
out appropriately.

2. Insert the filter paper into a beaker containing a small


volume of solvent. The depth of the solution should be
slightly lower than the reference line on the filter paper.

3. Leave the beaker and filter paper for a suitable time to allow
the solvent to migrate through the filter paper and enable
the chromatography process to occur. Keep the beaker in a
constant temperature away from direct sunlight to minimise
evaporation.

4. Remove the filter paper from the beaker and discard the
unused solvent.

Results

The pigments within ink will have separated and spread.

What can you conclude about the pigment that has travelled the
furthest?

Extended

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(/)
R
f
values  Help

Another method for identifying a substance using chromatography is to


()
find its
R
f
value (
Figure 3
).

The
R
f
value of a substance is the ratio of the distance moved by the
2.2 ()
substance (solute) compared to the overall distance moved by the
2.2.0 ()
solvent. Both distances are measured from the reference line. The
R
f
2.2.1 () value of any substance in a particular solvent is always the same

2.2.2 () provided that the chromatography techniques and conditions used to


obtain it are maintained. 
2.2.3 ()

The formula used to calculate


R
f
values is:

R
f
value =
\(\dfrac {\text{distance travelled by the solute}}{\text{distance
travelled by the solvent}}\)

The number generated will always be less than one because the distance
travelled by the solvent will always be greater than the distance
travelled by the solute.

Figure 3
. Diagram outlining how R
f
values can be obtained and
 calculated.
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The
R
f
value of a substance is always the same when a specific solvent is
()
used, but the same substance will have a different
R
f
value in a different
solvent. As a result, an individual substance will have multiple recorded
2.2 () R
f
values. While unlikely, two unknown solutes with the same
R
f
value

2.2.0 () may appear independently of one another on the same chromatogram.


In this case, the chromatography process is repeated using a different
2.2.1 ()
solvent.
2.2.2 ()

Once calculated, 
R
f
values can be compared to known standards
2.2.3 ()
published online and in reference books to identify the unknown
substance.

Locating agents
Identifying the constituent partitioned by paper chromatography of a
coloured substance such as ink or chlorophyll is a relatively simple
procedure because they can be seen clearly. Colourless substances, such
as amino acids, present an interesting conundrum. They can be
separated by chromatography (because this procedure is based on a
substance's solubility and mass) but identification is much more
challenging.

A locating agent is a chemical substance that will react with the solute(s)
separated by the chromatogram to produce a coloured substance. The
coloured substance will be clearly visible on the chromatogram. It can
then be positively identified by calculating its
R
f
value.

Ninhydrin is the name of the locating agent used to highlight the


position of individual amino acids after separation by paper
chromatography. The locating agent is sprayed onto the chromatogram

and then the paper is warmed in an oven for 10 minutes to allow the
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p p
(/) colours to develop. Each amino acid will be visible as either a purple
 Help
or a

yellow spot on the sheet of paper. The


R
f
value of each visible spot is
()
then calculated and compared to published values to enable
identification of the individual amino acids present.
2.2 ()

2.2.0 ()
 Study skills
2.2.1 ()
Different substances require different locating agents.
2.2.2 () Lists of locating agents used to identify individual
substances can be found in general chemistry reference
2.2.3 ()
books.

You do not need to be able to identify specific locating


agents, just recall their use.

Purity
Paper chromatography can be used to confirm the presence of and identify
impurities contained within an amount of substance. Impure substances
will leave more than the expected number of characteristic deposits on a
chromatogram.

Pure substances have experimentally defined


melting points
and
boiling points
known as
fixed points
.

Pure substances contain only one type of particle (atom or molecule). As a


result, the chemical bonds between the particles form and break at specific
temperatures. Impurities within a substance disrupt the original
arrangement of the particles and alter the temperature at which the bonds
between them form and break.

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Water provides us with an excellent illustration of how fixed points can be


()
altered by impurities. Pure water melts at 0 °C and boils at 100 °C, yet
seawater, which contains many impurities, freezes at approximately –2 °C
2.2 () and boils at approximately 101 °C.
2.2.0 ()

2.2.1 ()
 Study skills
2.2.2 ()
The purity of a substance is determined by the strength of the
2.2.3 () chemical bond formed between two particles and the amount of
energy required to bring about a change in state.

The nature of the chemical bonds that form between the particles
of a substance will be discussed in
subtopic 3.2
(/schoolstaff/app/cambridge-igcse-chemistry-2019/book/atoms-
elements-and-compounds/structure-and-bonding/the-big-
picture/)
.

The purity of a substance is crucial to its performance within a complex


substance, such as a pharmaceutical drug or foodstuff. Impurities can result
in unwanted and potentially lethal side effects or may impair the overall
quality of the final product.

  

Section questions
+ Show 4 questions


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(/) Section 2.2.2


 Help

() Methods of purification


 Students who have completed 24/24
this section (by class):
2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 () Methods of purification


2.2.3 ()

Solvents
A
solvent
is a liquid, such as water or ethanol, within which a substance,
called a
solute
, dissolves. Solvents are not universal. For example, sodium
chloride is very
soluble
in water but insoluble in ethanol. Mixtures of solid
substances are separated using solvents to create a
suspension
that can be
filtered. 

Ethanol, for example, can be used to separate two solids such as sugar and
salt (sodium chloride) within a mixture (
Figure 1
). Added to the solid
mixture, ethanol creates a suspension within which the sugar has dissolved
but not the salt. Filtration of the suspension produces a filtrate of sugar
dissolved in ethanol and leaves a residue of salt. Sugar is obtained from the
filtrate by simply allowing the ethanol to evaporate.


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()

2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 ()

2.2.3 ()

Figure 1
. Using a solvent to separate two solids.

Filtration
Filtration
is a very simple technique used to separate an
insoluble
solid
from a liquid within a suspension.

Filtration classically requires the use of a filter funnel (


Figure 2
). An
insoluble solid material separates from the liquid because it is unable to
pass through the small hole at the base of the funnel. Frequently, however,
an additional
filter paper
is required to decrease the size of the hole(s)
through which the suspension passes. This enables fine suspensions such
as ground coffee and water to be separated.


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()

2.2 ()

2.2.0 ()

Credit: GI15606757 iStock
2.2.1 ()

2.2.2 ()

2.2.3 () Figure 2
. Filtration of an insoluble solid from a liquid.

Filtration can be used to remove unwanted substances from a suspension,


leaving a pure filtrate, or to obtain a particular solid from a solution.

Crystallisation
A crystal is a small, regularly shaped solid that reflects light. Salt (sodium
chloride) and diamond are good examples. Crystals are soluble and
dissolve in a solvent to produce a solution. Many crystals, for example
copper sulfate, dissolve in water to produce coloured solutions (
Figure 3
).


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()

2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 ()
Credit: Nneirda iStock Credit: tarasov_vl iStock
2.2.3 ()

Figure 3
. Crystals of copper sulfate have a small, regular shape that reflects
light. These crystals will dissolve in water forming copper sulfate solution.

Crystallisation
is a method that allows pure crystals of a particular solid to
be obtained from a solution as it cools (
Figure 4
). As the temperature of a
solution decreases, less space is available within the liquid for the solid
particles. These particles are pushed out and gradually grow as crystals on
the sides of the container holding the solution. If a liquid solution is
allowed to cool slowly, the crystals grown will be much larger than those
formed from rapid cooling.


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()

2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 ()

2.2.3 ()
Figure 4
. A method for crystallisation to separate copper sulfate crystals from
a solution.

Watch this video to see crystals growing from a solution.

Crystal Time Lapse (Canon 550D)

Distillation

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The separation of a liquid from another liquid within a solution is difficult


()
compared to the simple separation of an insoluble solid from a liquid in
suspension.
Distillation
is a separating technique used to separate liquids
2.2 () by temporarily transforming one of the liquids into a gas.
2.2.0 ()
Simple distillation is used to obtain a solvent from a solution. The process
2.2.1 ()
of simple distillation uses a round bottomed flask connected to a long tube,
2.2.2 ()
called a condenser, through which cold water flows (
Figure 5
).
2.2.3 ()

Credit: Airubon iStock

Figure 5
. Apparatus for distillation.

The essential principles of simple distillation are outlined below.

The original solution is heated within the round bottomed flask.


One of the liquids boils (at the lower boiling point) and changes state
to gas.
The vapour passes along the condenser. Cold water running through
 the condenser acts as a heat exchanger, absorbing heat energy from
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the gas, which in turn cools the gas back into a liquid and this is
()
collected in the beaker.
The other liquid, which has a higher boiling point, is left behind in the
2.2 () round bottomed flask.
2.2.0 ()
Simple distillation uses the fact that different substances have varying
2.2.1 ()
fixed points (for example, boiling points). In a mixture, a liquid with a
2.2.2 ()
lower boiling point will change the state to a gas before one with a higher
2.2.3 () boiling point. Simple distillation is used to separate a mixture of liquids
whose boiling point temperature difference is at least 50 °C.

Fractional distillation
is used to separate a mixture of liquids whose boiling
points are approximately within 25 °C of each other. In the case of crude
oil, for example, component hydrocarbons such as petrol and paraffin have
similar boiling points and so fractional distillation is carried out rather than
simple distillation.

When carried out in a school laboratory, the apparatus required for


fractional distillation is similar to that used in simple distillation. However,
the column or neck of the round bottom flask differs from that used in
simple distillation in that it contains glass beads that control the
temperature within the column (
Figure 6
).


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()

2.2 ()

2.2.0 ()

2.2.1 ()

2.2.2 ()

2.2.3 ()

Figure 6
. Laboratory fractional distillation equipment.

When the mixture of liquids in the round bottom flask is heated, both
substances will start to vaporise because of their similar boiling points. The
beads provide a cool surface over which the vapour from the liquid with
the highest boiling point will condense and then drop back into the flask,
while the other liquid moves through to the top of the column and then into
the condenser.

 Study skills
Fractional distillation is used industrially to separate crude oil into
 its different constituents and to purify the alcohol (ethanol)
produced by fermentation for use as a solvent fuel and in drinks
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produced by fermentation for use as a solvent, fuel and in drinks
(/) such as whiskey. We will study these applications of fractional
 Help

distillation in
subtopics 14.2
(/schoolstaff/app/cambridge-igcse-
() chemistry-2019/book/organic-chemestry/fuels/the-big-picture/)
and
14.6
(/schoolstaff/app/cambridge-igcse-chemistry-
2019/book/organic-chemestry/alcohols/the-big-picture/)
.
2.2 ()

2.2.0 ()

2.2.1 ()   

2.2.2 ()
Section questions
2.2.3 () + Show 4 questions

Section 2.2.3

Checklist
 Students who have completed 21/24
this section (by class):

 What you should know

By the end of this subtopic 2.2 Purity, you should be able to:

Core

Demonstrate knowledge and understanding of paper


chromatography.

Interpret simple chromatograms.


Identify substances and assess their purity from melting
 point and boiling point information.
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Understand the importance of purity in substances in


() everyday life, e.g. foodstuffs and drugs.

Describe and explain methods of purification by the use of a


suitable solvent, filtration, crystallisation and distillation
2.2 ()
(including use of a fractionating column).
2.2.0 ()
Suggest suitable purification techniques, given information
2.2.1 () about the substances involved.

2.2.2 ()  Supplement

2.2.3 () Interpret simple chromatograms, including the use of Rf


values.
Outline how chromatography techniques can be applied to
colourless substances by exposing chromatograms to
substances called locating agents.

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