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5.6.5Unit 5. Transition Metals and Organic Nitrogen Chemistry

Organic Techniques – Purification — IAL Edexcel Linear (Chemistry) Revision Notes & Topical Questions

5 min read 4 parts Lesson 42 of 43 Unit quiz

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Curriculum Equation Key قوانين الرقم الهيدروجيني والاتزان الأيوني - pH & Acid-Base Equilibrium FormulasFast Exam Solution
pH = -log[H⁺] | pOH = -log[OH⁻] | pH + pOH = 14 | [H⁺][OH⁻] = 10⁻¹⁴
Word Equation & Conditions: الرقم الهيدروجيني = -لوغاريتم تركيز أيون الهيدروجين | pH + pOH = 14
Location & Specifications: الاتزان الأيوني، كيمياء 3 ثانوي، التحصيلي، و AP Chemistry.
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Part 1 of 4Purifying a Liquid Product

1
Transfer the cooled distillate to a separating funnel and add water or a wash solution so two layers form.
2
Run off the lower layer, working out which layer contains the organic product from its density relative to water.
3
Wash the organic layer with sodium hydrogencarbonate solution to remove acidic impurities; carbon dioxide forms, so open the tap often to release pressure.
4
Dry the organic layer with an anhydrous drying agent such as anhydrous magnesium sulfate or calcium chloride until it is no longer cloudy.
5
Filter off the drying agent and redistil the liquid, collecting only the fraction at the correct boiling point.

Part 2 of 4Separating Funnel and Drying

Water and acid are the commonest impurities in a liquid product.

Immiscible layers
  • Immiscible layers The organic layer and the aqueous layer do not mix, so they can be separated by running off one layer.
Why wash
  • Why wash Sodium hydrogencarbonate reacts with acid impurity: RCOOH + NaHCO₃ → RCOONa + H₂O + CO₂.
Drying agent
  • Drying agent Anhydrous salts take up traces of dissolved water by forming hydrates and are easily removed by filtration.
Sign of dryness
  • Sign of dryness The liquid turns from cloudy to clear and some of the solid drying agent stays free-flowing.

Part 3 of 4Purifying a Solid by Recrystallisation

Purifying a Solid by Recrystallisation
Choose solvent
  • Choose solvent The solid should dissolve well in the hot solvent but poorly in the cold solvent.
Dissolve
  • Dissolve Add the minimum volume of hot solvent so that the solution is saturated and the maximum yield is recovered.
Hot filtration
  • Hot filtration Filtering while hot removes insoluble impurities before the product starts to crystallise.
Cool and collect
  • Cool and collect Slow cooling gives larger purer crystals, which are filtered under reduced pressure and washed with a little cold solvent.
MethodBest forRemoves
RedistillationLiquidsImpurities of different boiling point
RecrystallisationSolidsSoluble and insoluble impurities
Solvent extractionMixtures in two solventsWater-soluble or acid impurities

Part 4 of 4Exam Checklist & Tips

5.6.5 – Key Points for the Exam

  • Immiscible Liquids that do not mix and form two separate layers.
  • Drying agent An anhydrous solid added to remove traces of water from a liquid.
  • Recrystallisation Purification of a solid by dissolving in hot solvent and cooling to form crystals.
  • Filtration under reduced pressure Faster filtration using a vacuum with a Buchner funnel.

Common Mistakes

  • Using too much hot solvent in recrystallisation, which lowers the yield.
  • Failing to vent the separating funnel when washing with carbonate, so pressure builds up.
  • Using a wet or hydrated drying agent that cannot remove more water.
  • Washing crystals with warm solvent, which dissolves some product.

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