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Exam Question – 4 marks

A student was given three compounds, an aldehyde, a


ketone, and a carboxylic acid.
The student carried out the same two chemical tests on
each compound. This allowed her to distinguish between all
three compounds.
• Describe two suitable tests that the student could have used.
• Show how the observations would allow her to distinguish
between the compounds.
Exam Question
6.3.1.1 Chromatography
Objective:
Explain how different types of chromatography work.
Outcomes:
• Describe how chromatography works in terms of mobile and
stationary phases.
• Explain how the interactions of mobile and stationary phases
causes separation.
• Evaluate the use of different types of chromatography.
Specification Links:
Unit: 6. Organic Chemistry & Analysis
Module: 3. Analysis
Topic: 1. Chromatography & Qualitative Analysis
Specification Links
4.3.1 Types of Chromatography
a. Interpret one-way TLC chromatograms in terms of Rf­ values.
b. Interpret gas chromatograms in terms of:
i. Retention times.
ii. The amounts and proportions of the components in a
mixture.
Chromatography
Chromatography is a technique used to separate
components with similar physical properties from a
mixture.
To do this a mobile phase is passed over a stationary phase
and each compound has a different affinity for each phase.
• A phase is a physically distinct form of a substance.

The stationary phase slows compound movement and the


more interactions there are the more it is slowed down.
• This allows compounds to move at different rates.
Separation
Solid Stationary Phase Liquid Stationary Phase
Separate by adsorption as Separate by relative solubility as
molecules bind on to the surface. molecules dissolve into the
phase.

Stronger adsorption = slower.


Greater solubility = slower.
Thin-Layer Chromatography (TLC)
A stationary phase of silica gel (SiO2) or alumina (Al2O3) is
coated onto a plate of glass or plastic.
A sample is added to a starting point on the plate which is
then placed into a liquid solvent which will get drawn up.
• At the end the height of the solvent is marked – the solvent
front.
Rf Values
An Rf value shows how far a component has moved relative
to the solvent front:
distance moved by component
Rf 
distance moved by solvent front

This can identify a component as it will always have the


same Rf values, however:
• Similar compounds may have the similar Rf values.
• A suitable solvent is needed to separate the different compounds.
Rf Values
Calculate the values for each of these components three
components.

4.30
Rf   0.89
4.85

Y = 4.85 cm
Green = 1.65 cm Rf 
2.15
 0.44
4.85
Pink = 2.15 cm 1.65
Rf   0.34
Blue = 4.30 cm 4.85
Gas Chromatography
A stationary phase of solid silicone polymers or a liquid long
chain alkane (w/ high B.P.) is coated inside a capillary tube.

A sample is injected and vaporised before being pushed


through the capillary column by a carrier gas (mobile phase).
• An inert/unreactive gas such as He or N2.
Retention Time
The detector at the end records how long it took for a
component to pass through the column (retention time).
• The area below a peak is proportional to the concentration.

The retention time can help identify the component but:


• Chemicals can have the same retention
time, peak shape and detector response.
• One peak can be hidden by others with
the same retention time but a greater
concentration.

To improve results chromatography is often paired with


mass spectroscopy (GC-MS).
High-Performance Liquid Chromatography
(HPLC)

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