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Development of Practical Skills in Chemistry

Reflux, distillation, purification and the standard tests

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Overview

Recall questions on reflux and distillation, separating and drying an organic layer, recrystallisation, melting point, Rf values and the standard test-tube tests.

What you need to know

Answer each one before you reveal it.

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Key term

How is a separating funnel used to purify an organic liquid, and what precaution must be taken?

Questions from this subtopic

Each one with the model answer underneath.

  1. 1

    What does heating under reflux achieve, and why is the condenser vertical and open at the top?

    Model answer

    It allows a mixture to be boiled for a long period without loss of volatile material, because vapour condenses and runs back into the flask; the top is left open so pressure cannot build up, and anti-bumping granules are added so that boiling is smooth rather than violent.

  2. 2

    In a simple distillation, where must the thermometer bulb be placed and why?

    Model answer

    The bulb sits level with the side arm leading to the condenser so that it measures the temperature of the vapour actually passing over.

  3. 3

    How is a separating funnel used to purify an organic liquid, and what precaution must be taken?

    Model answer

    The mixture is shaken in the stoppered funnel, the layers allowed to settle, and the lower layer run off through the tap; the funnel must be inverted and the tap opened during shaking to release the pressure of any vapour or gas.

  4. 4

    Which drying agent is added to a separated organic layer, and how do you know enough has been used?

    Model answer

    Anhydrous magnesium sulfate or sodium sulfate is added, and enough has been used when some of the solid remains as a free-running powder rather than clumping together.

  5. 5

    How is a solid purified by recrystallisation, and why is the minimum volume of hot solvent used?

    Model answer

    The impure solid is dissolved in the minimum volume of hot solvent, filtered hot, then cooled so that crystals of the product form and are filtered off; using the minimum volume ensures the solution is saturated so that the maximum amount of product crystallises on cooling.

  6. 6

    Why is a fluted filter paper used for hot filtration during recrystallisation?

    Model answer

    The folds increase the surface area available so the hot solution passes through quickly, before it can cool and deposit crystals in the funnel.

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A acid is formed.
carboxylicnitricfatty

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A3 ⁴₂He → ¹²₆C.
B¹²₆C + ⁴₂He → ¹⁶₈O.
C¹⁶₈O + ⁴₂He → ²⁰₁₀Ne.

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Nitrogen is +2 in NO and +4 in NO₂.
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