ANALYSING

SUBSTANCES
A guide for GCSE students

KNOCKHARDY PUBLISHING

2010

SPECIFICATIONS

ANALYSING SUBSTANCES
INTRODUCTION
This Powerpoint show is one of several produced to help students
understand selected GCSE Chemistry topics. It is based on the requirements
of the AQA specification but is suitable for other examination boards.
Individual students may use the material at home for revision purposes and
it can also prove useful for classroom teaching with an interactive white
board.
Accompanying notes on this, and the full range of AS and A2 Chemistry
topics, are available from the KNOCKHARDY WEBSITE at...

www.knockhardy.org.uk

All diagrams, photographs and any animations in this Powerpoint are

original and created by Jonathan Hopton. Permission must be
obtained for their use in any work that is distributed for financial gain.
HOPTON

ANALYSING SUBSTANCES
CONTENTS
What is chromatography?
Paper chromatography
Gas liquid chromatography
Mass spectrometry
Questions

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CHROMATOGRAPHY
Chromatography is used to separate and analyse small amounts of mixtures

HOPTON

CHROMATOGRAPHY
Chromatography is used to separate and analyse small amounts of mixtures
Methods involve a
and a

stationary phase
mobile phase

There are several forms of chromatography

HOPTON

(stays where it is)

(moves)

CHROMATOGRAPHY
Chromatography is used to separate and analyse small amounts of mixtures
Methods involve a
and a

stationary phase
mobile phase

(stays where it is)

(moves)

There are several forms of chromatography

TYPE

STATIONARY PHASE

MOBILE PHASE

paper

solid (filter paper)

liquid

thin layer (tlc)

solid (silica)

liquid

column

solid (silica)

liquid

solid or liquid

gas

gas liquid (glc)

However, they all work in the same way

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PAPER CHROMATOGRAPHY

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PAPER CHROMATOGRAPHY
Stationary phase

chromatography paper

Mobile phase

suitable solvent (water, ethanol, organic solvent)

HOPTON

PAPER CHROMATOGRAPHY
Stationary phase

chromatography paper

Mobile phase

suitable solvent (water, ethanol, organic solvent)

Separation

As the solvent moves up the paper it dissolves the

components and moves them up the paper. The
more soluble a component is, the further it moves.

HOPTON

PAPER CHROMATOGRAPHY
Stationary phase

chromatography paper

Mobile phase

suitable solvent (water, ethanol, organic solvent)

Separation

As the solvent moves up the paper it dissolves the

components and moves them up the paper. The
more soluble a component is, the further it moves.

Uses

Separating the colours in Smarties

Separating the colours in, and identifying, inks

HOPTON

PAPER CHROMATOGRAPHY
Stationary phase

chromatography paper

Mobile phase

suitable solvent (water, ethanol, organic solvent)

Separation

As the solvent moves up the paper it dissolves the

components and moves them up the paper. The
more soluble a component is, the further it moves.

Place small a spot of the mixture

to be analysed (and any possible
component for comparison
purposes) on the paper. Dip the
paper in the solvent.

HOPTON

PAPER CHROMATOGRAPHY
Stationary phase

chromatography paper

Mobile phase

suitable solvent (water, ethanol, organic solvent)

Separation

As the solvent moves up the paper it dissolves the

components and moves them up the paper. The
more soluble a component is, the further it moves.
SOLVENT
FRONT

Place small a spot of the mixture

to be analysed (and any possible
component for comparison
purposes) on the paper. Dip the
paper in the solvent.

Allow the solvent to rise up the

paper. Each component
dissolves in the solvent. Those
which are more soluble travel
further up the paper.
HOPTON

PAPER CHROMATOGRAPHY
Stationary phase

chromatography paper

Mobile phase

suitable solvent (water, ethanol, organic solvent)

Separation

As the solvent moves up the paper it dissolves the

components and moves them up the paper. The
more soluble a component is, the further it moves.
SOLVENT
FRONT

Place small a spot of the mixture

to be analysed (and any possible
component for comparison
purposes) on the paper. Dip the
paper in the solvent.

Allow the solvent to rise up the

paper. Each component
dissolves in the solvent. Those
which are more soluble travel
further up the paper.
HOPTON

Finished
chromatogram

PAPER CHROMATOGRAPHY
Rf value

Under similar conditions, a component

should always travel at the same speed.

SOLVENT
FRONT

Its identity can be found by comparing

the distance it moves relative to the solvent.
X
Rf = distance travelled by the component
distance travelled by the solvent

HOPTON

Y
X

PAPER CHROMATOGRAPHY
Rf value

Under similar conditions, a component

should always travel at the same speed.
Its identity can be found by comparing
the distance it moves relative to the solvent.
X
Rf = distance travelled by the component
distance travelled by the solvent

Comparison can be a problem if

a) components have similar Rf values
b) the unknown substance is new and there is
no previous chemical to compare it with

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Y
X

GAS LIQUID CHROMATOGRAPHY (GLC)

HOPTON

GAS LIQUID CHROMATOGRAPHY (GLC)

Stationary phase

liquid adsorbed onto a solid support material

Mobile phase

gas

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GAS LIQUID CHROMATOGRAPHY (GLC)

Stationary phase

liquid adsorbed onto a solid support material

Mobile phase

gas

Method
a very small amount of a sample
is injected into the machine
the injector is contained in an oven
the sample boils and is carried along
a thin column by an inert carrier gas

HOPTON

GAS LIQUID CHROMATOGRAPHY (GLC)

Stationary phase

liquid adsorbed onto a solid support material

Mobile phase

gas

Method
a very small amount of a sample
is injected into the machine
the injector is contained in an oven
the sample boils and is carried along
a thin column by an inert carrier gas
the column contains a liquid stationary phase, adsorbed on an inert solid
the time taken to travel through the tube will depend on how much time is
spent moving with the gas rather than being attached to the liquid.

HOPTON

GAS LIQUID CHROMATOGRAPHY (GLC)

Retention time

The time taken for a compound to travel through the

column to the detector.
It is measured from the time the sample is injected to
the time its peak shows maximum height.

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GAS LIQUID CHROMATOGRAPHY (GLC)

Retention time

The time taken for a compound to travel through the

column to the detector.
It is measured from the time the sample is injected to
the time its peak shows maximum height.
For a particular compound, the retention time depends on...
boiling point

high boiling point = long retention time

HOPTON

GAS LIQUID CHROMATOGRAPHY (GLC)

Retention time

The time taken for a compound to travel through the

column to the detector.
It is measured from the time the sample is injected to
the time its peak shows maximum height.
For a particular compound, the retention time depends on...
boiling point

solubility in the liquid phase

high boiling point = long retention time

greater solubility = long retention time

HOPTON

GAS LIQUID CHROMATOGRAPHY (GLC)

Retention time

The time taken for a compound to travel through the

column to the detector.
It is measured from the time the sample is injected to
the time its peak shows maximum height.
For a particular compound, the retention time depends on...
boiling point

solubility in the liquid phase

high boiling point = long retention time

greater solubility = long retention time
ANIMATION

HOPTON

GAS LIQUID CHROMATOGRAPHY (GLC)

Interpretation
each compound in the mixture will produce a peak
the areas under the peaks are proportional to the amount of a compound
retention times are used to identify compounds they are found out by
putting known compounds through the system under similar conditions

The area under a

peak is proportional
to the amount
present.

Because each compound

responds differently, the
machine is calibrated
beforehand to show the
actual mount.

Each component has a different retention time.

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GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

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GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer

HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
Mass spectrometers were first used to identify the
presence of different isotopes.
Today, they are mainly used to work out relative molecular
(formula) mass and identify unknown molecules.

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GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer

HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...

HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...
ANALYSER
IONISER

HOPTON

DETECTOR

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...
ANALYSER

DETECTOR

IONISER

Ioniser

- the sample is bombarded with electrons and ionised

- a positive molecular ion is formed
- the molecular ion can break up into smaller ions

PARTICLES MUST BE IONISED SO THEY

CAN BE ACCELERATED AND DEFLECTED
HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...
ANALYSER

DETECTOR

IONISER

Ioniser

the sample is bombarded with electrons and ionised

a positive molecular ion is formed
the molecular ion can break up into smaller ions
positive ions are accelerated towards the analyser

HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...
ANALYSER

DETECTOR

IONISER

Ioniser

the sample is bombarded with electrons and ionised

a positive molecular ion is formed
the molecular ion can break up into smaller ions
positive ions are accelerated towards the analyser

Analyser

- positive ions separate according to mass/charge ratio

- higher mass/charge ratio (heavier) = smaller deflection

HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...
ANALYSER

DETECTOR

IONISER

Ioniser

the sample is bombarded with electrons and ionised

a positive molecular ion is formed
the molecular ion can break up into smaller ions
positive ions are accelerated towards the analyser

Analyser

- positive ions separate according to mass/charge ratio

- higher mass/charge ratio (heavier) = smaller deflection

Detector

- records the identity and abundance of each ion

- compounds have a unique mass spectrum
- the final peak (molecular
ion) gives the molecular mass
HOPTON

GAS CHROMATOGRAPHY MASS SPECTROMETRY (GCMS)

Process

When a peak is detected in gas chromatography, some of

the component is sent to a mass spectrometer
A mass spectrometer has three main parts...
ANALYSER

DETECTOR

IONISER

Ioniser

the sample is bombarded with electrons and ionised

a positive molecular ion is formed
the molecular ion can break up into smaller ions
positive ions are accelerated towards the analyser

Analyser

- positive ions separate according to mass/charge ratio

- higher mass/charge ratio (heavier) = smaller deflection

Detector

- records the identity and abundance of each ion

- compounds have a unique mass spectrum
- the final peak (molecular
ion) gives the molecular mass
HOPTON

MASS SPECTROMETRY - FRAGMENTATION

Mass spectrometry is used to identify
unknown or new compounds.
The mass spectra of compounds are much
more complicated than that of atoms
because of fragmentation.

IONISATION

MOLECULAR ION

When a molecule is ionised it forms a

MOLECULAR ION which can undergo
FRAGMENTATION or RE-ARRANGEMENT
to produce particles of smaller mass.

FRAGMENTION

RE-ARRANGEMENT

FRAGMENTION

Only particles
with a positive charge
will be deflected and detected.
The resulting spectrum has many peaks.
The final peak shows the molecular ion
and indicates the molecular mass. The rest
of the spectrum provides information
about the structure.
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QUESTIONS

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MASS SPECTRUM OF AN ORGANIC COMPOUND

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MASS SPECTRUM OF AN ORGANIC COMPOUND

Which signal is caused

by the molecular ion?

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MASS SPECTRUM OF AN ORGANIC COMPOUND

The final signal

in the spectrum
is that of the
molecular ion.

Which signal is caused

by the molecular ion?

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MASS SPECTRUM OF AN ORGANIC COMPOUND

What is the relative molecular

(formula) mass of the compound?
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MASS SPECTRUM OF AN ORGANIC COMPOUND

58

What is the relative molecular

(formula) mass of the compound?
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MASS SPECTRUM OF AN ORGANIC COMPOUND

If the compound is a hydrocarbon,

what is its molecular formula?
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MASS SPECTRUM OF AN ORGANIC COMPOUND

What is the relative molecular

(formula) mass of the compound?
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C4H10

ANALYSING
SUBSTANCES
THE END

2011 JONATHAN HOPTON & KNOCKHARDY PUBLISHING