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Separation and Purification

Pure Substances
1. A pure substance contains only one type of substance and isn't mixed with any
other substances. It can be an element or a compound, consisting of one type of
atom or molecule. Examples include nitrogen gas and sodium chloride crystals.

2. Criteria for a substance to be considered pure:

Fixed melting point (melts at a fixed temperature). For example, ice melts
at 0 °C at atmospheric pressure.
Fixed boiling point. For example, pure ethanol boils at 78 °C at
atmospheric pressure.

A fixed temperature can also be described as a sharp and constant

temperature.

3. Impurities affect the melting and boiling points of a pure substance:

Impurities lower the melting point and cause the substance to melt over
a range of temperatures. For example, adding salt to ice causes the
mixture to melt between –5 °C to –25 °C.
Impurities raise the boiling point and cause the substance to boil over a
range of temperatures. For example, seawater boils over a range of 101
°C to 103 °C.

4. Purity of a substance can be determined by:

Checking the melting temperature of a solid.

Checking the boiling temperature of a liquid.
Performing chromatography.

Physical Methods of Separation

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1. A mixture is when two or more substances are present but are not chemically
joined together. Mixtures are not pure substances.

2. Physical methods can be used to separate the pure substances in a mixture

without causing any chemical changes.

3. The method of separation depends on the physical properties of the

components.

Separating an Insoluble Solid from a Liquid

1. Filtration is used to separate an insoluble solid from a liquid. An example is
sand and water. When the mixture is filtered:

The solid left behind on the filter paper is the residue.

The liquid that passes through the filter paper is the filtrate.

Filter paper has tiny pores that only allow dissolved substances and liquid to
pass through; insoluble solids are too large to pass through.

Example: A sample of sand is contaminated with table salt:

Add excess water to dissolve all the salt.

Filter the mixture and collect the filtrate.
Evaporate the filtrate to dryness to obtain dry table salt.

2. Decanting is sufficient if the insoluble particles are large and heavy enough.
The mixture is separated into two distinct layers: the liquid on top and the
sediment (solid) at the bottom. The liquid layer is then poured off carefully
without disturbing the sediment. Decanting is faster but less efficient than
filtration.

3. Centrifugation can be used when insoluble particles are fine and suspended in
the liquid. The suspension in a test tube is placed in a centrifuge, which rotates
at high speed. This draws the fine particles to the bottom of the test tube.

Separating a Soluble Solid from a Liquid

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1. Evaporation to dryness is when the mixture is heated to evaporate the

solution. The solid remains as a residue after the solvent has evaporated. A
water bath is used if the liquid in the mixture is flammable (e.g., ethanol).

Disadvantage: If any other soluble impurities are present in the solution, the
solid obtained will not be pure because only the liquid evaporates, leaving all
other solids behind.

2. Crystallization is used to obtain solids that are unstable to heat, as evaporation

to dryness is not suitable for solids that decompose upon heating (e.g., sugar
decomposes to carbon upon heating).

Process: The solution is heated to boil off some of the solvent to make the
solution saturated, then allowed to cool. As the solution cools, crystals of solid
appear, which are pure as the impurities remain dissolved in the solution.

A saturated solution is a solution that contains the maximum

amount of solute at a given temperature. If more solid is added, it
will not dissolve.

Crystallization is used:

If the solid crystals decompose when the solution is heated to dryness.

Only for compounds whose solubilities vary greatly with temperature.

Crystallization is not suitable to be used on sodium chloride. To obtain large

and well-defined crystals, the aqueous solution must be cooled slowly.

Separating a Liquid from a Solution

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1. Simple distillation is used to obtain the solvent from a solution.

Example: Recovering water from seawater.

Process: The solution is heated to its boiling point, and the solvent changes into
a vapor, leaving other substances behind in the flask. The vapor is cooled by a
condenser (Liebig condenser) and changed back into a liquid, called a distillate.

Boiling chips are added to ensure smooth boiling by allowing the

formation of smaller air bubbles.
A thermometer is placed near the opening of the condenser to measure
the temperature of the vapor exiting the flask. The thermometer shows a
constant temperature when the liquid is being distilled, indicating the
boiling point of the vapor.
Cooling water enters the bottom of the condenser to ensure that the
bottom is the coolest part, allowing effective condensation of the vapor.

2. Fractional distillation is used to separate two or more miscible liquids with

different boiling points.

Miscible means that the liquids can dissolve in each other.

The fractionating column is usually packed with glass beads to provide a large
surface area for condensation of vapor, so the components with different boiling
points will leave the column at different times, ensuring effective separation of
liquids. The liquid with the lowest boiling point is distilled first, while the liquid
with the highest boiling point is distilled last.

Example: A mixture of water (b.p. = 100 °C) and ethanol (b.p. = 78 °C).

Process:

1. Ethanol vapor and water vapor rise up the column as the solution is
heated.
2. When the temperature at the top of the column reaches 78 °C, ethanol
vapor passes into the condenser. Water vapor, with the higher boiling
point, condenses out and returns into the flask.
3. Ethanol vapor condenses as it passes through the condenser and is
collected as the distillate.

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The thermometer first records the temperature of the ethanol vapor, which is
78 °C. After all the ethanol vapor has entered the condenser, the thermometer
will then record the temperature of the steam, which is 100 °C.

Fractional distillation is commonly used for:

Separation of pure nitrogen and oxygen in liquid air.

Separation of fractions in crude oil.
Separation of ethanol from fermented solution.

Separating Immiscible Liquids

Some liquids do not mix and tend to separate into distinct layers, these are
immiscible liquids. An example is oil and water. A separating funnel is used to
separate the liquids. The lower layer (liquid of higher density) can be drained off first
using the tap.

Separating Solids from a Mixture of Solids

Sublimation is when some solids can change into a gas directly without going
through the liquid state. Examples of solids that sublime:

Iodine
Dry ice (solid carbon dioxide)
Naphthalene (mothball)

Example: Separating a mixture of naphthalene and sodium chloride.

Heat the mixture in an evaporating dish and invert a filter funnel over the
mixture.
Naphthalene sublimes, and the vapor deposits on the cool surface of the filter
funnel.

Chromatography

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1. Chromatography is a technique that uses a solvent to separate a mixture into

its components. The components need to be soluble in the same solvent.

2. Chromatography can be used to:

Determine if a sample is pure.

Separate the components in a sample.
Identify the components present in a sample.

Procedure for Paper Chromatography

1. Draw a pencil line on a piece of chromatography paper.
2. Put a tiny spot of the sample on the pencil line. Pencil is used instead of ink
because ink will dissolve in the solvent. The spot should be as small as
possible for good separation.
3. Dip the chromatography paper into the solvent. The spot is above the initial
level of solvent to prevent the sample from dissolving completely in the
solvent.
4. The solvent is absorbed by the paper and rises up. The components in the
sample dissolve in the solvent and move up the paper at different speeds.
5. Remove the chromatography paper when the solvent has reached near the top
edge of the paper. The resulting chromatography paper with the separated
spots of colors is called a chromatogram.

A component that is more soluble in the solvent will travel faster and further across
the paper. Others are less soluble in the solvent and therefore do not travel very far
across the paper. This difference in solubility allows the different components in a
sample to be separated. Identical components will travel the same distance up the
chromatography paper.

The separation of components in paper chromatography depends on the

relative solubilities of the components in two different substances, one
that is not moving (called the stationary phase) and the other that is
moving (called the mobile phase).

Interpretation of Chromatogram

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The number of spots indicate the number of components in the sample.

A substance with one single spot is pure.
A substance with multiple spots is impure and consists of multiple
components.
Identical components produce spots at the same height. Hence, we can
compare the positions of components on the chromatogram.
Identity of a spot can be obtained by comparing it to retention factor (R ) values
f

of known pure substances. R value is constant if the temperature is constant

f

and the solvent is fixed.

Distance travelled by solute (spot)
Rf =
Distance travelled by solvent

Example: The components of a sugar solution were separated using chromatography.

Sugar Rf value

Sucrose 0.20
Maltose 0.40
Glucose 0.57
Galactose 0.69
Fructose 0.86

If the distance traveled by Unknown Substance 1 is 2.5 and the distance traveled by
the solvent is 6.2, then the R value can be calculated.
f

2.5
Rf = = 0.403 ≈ 0.40
6.2

If the distance traveled by Unknown Substance 2 is 5.3 and the distance traveled by
the solvent is 6.2, then the R value can be calculated.
f

5.3
Rf = = 0.855 ≈ 0.86
6.2

Hence, the substances present are maltose and fructose.

Applications of Chromatography

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To separate dyes in ink.

To separate mixtures of pigments from plants, dyes from inks.
To separate amino acids obtained from proteins.
To identify poison or drugs or unlawful dyes in urine samples.
To detect impurities or monitor additives in food items.

How do we identify colorless substances (e.g., amino acids) using chromatography? A

locating agent is applied to the chromatogram. The locating agent reacts with the
substances to form colored products and enable the identification of substances.

Advantages of Chromatography
Only tiny amounts of the substances are needed.
Results can be quickly obtained.

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