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12.4Experimental Techniques and Chemical Analysis

Separation and purification — Cambridge IGCSE Chemistry 0620 Revision Notes & Topical Questions

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Lesson summary

12.4 Separation and purification — Notes — IGCSE Chemistry notes: Assess the purity of a substance and choose and describe methods of separating mixtures.TermMeaningExampleSolventThe liquid in which a solute dissolvesWater in sea waterSoluteThe substance that dissolves in a liqui…

  • Saturated solution
  • Crystallisation
  • Simple distillation
  • Fractional distillation
  • Pure substance
  • Mixture: melts and boils over a range of temperatures because its components change state at different temperatures

Section 1 of 11Terms used for solutions

TermMeaningExample
SolventThe liquid in which a solute dissolvesWater in sea water
SoluteThe substance that dissolves in a liquid to form a solutionSalt in sea water
SolutionMixture formed when a solute dissolves in a solventSea water
Saturated solutionMaximum concentration of solute dissolved at a given temperatureDead Sea water
Soluble / insolubleWill / will not dissolveSalt / sand in water
FiltrateLiquid or solution that has passed through a filterCoffee in a cup
ResidueSubstance remaining after evaporation, distillation, filtration or a similar processCoffee grounds in filter paper

Section 2 of 11Assessing purity

1
Pure substance: melts and boils at specific, sharp temperatures (water: melts at 0 °C, boils at 100 °C).
2
Mixture: melts and boils over a range of temperatures because its components change state at different temperatures.
3
Melting and boiling data show whether a sample is pure or a mixture.
4
Identifying a substance: measure its melting and boiling points and compare them with literature values or data tables.
  • Reference boiling points are quoted at a given pressure, so compare under the same conditions.
  • Boiling points are commonly found by distillation and melting points with a melting point apparatus.
5
Effect of impurities: the melting point appears lower and the boiling point appears higher than the true values.
6
The closer the measured value is to the true value, the purer the sample.

Section 3 of 11Measuring melting point

Measuring melting point
Method
  • Place a small sample in the melting point apparatus.
  • Heat it slowly so the thermometer and sample stay at nearly the same temperature.
  • Record the temperature at which melting starts and finishes.
  • Compare the range with the data-table value.
Melting point is routinely used to assess the purity of drugs.

Section 4 of 11Filtration

1
All separation techniques rely on a difference in a physical property such as solubility or boiling point.
2
Filtration separates an undissolved solid from a liquid or solution, such as sand from sand and water.
3
Large solid particles cannot pass through the filter paper and stay behind as the residue,
  • and the liquid or solution that passes through is the filtrate.
4
Centrifugation can also separate an undissolved solid from a liquid.
5
Separating two solids: dissolve the soluble one in a suitable solvent, filter off the insoluble one, then crystallise the filtrate.
6
Water dissolves salt but not sand.

Section 5 of 11Crystallisation

Crystallisation
Method
  • Heat the solution to evaporate some of the solvent, removing no more than about half, until it is saturated.
  • Test for saturation by dipping a clean, dry, cold glass rod in, as crystals form on the rod as it cools.
  • Leave the saturated solution to cool slowly so crystals grow as solubility falls.
  • Collect the crystals by filtration.
  • Wash the crystals with a little cold distilled water to remove impurities.
  • Dry them between sheets of filter paper or in a drying oven.
Use: for solids more soluble in hot solvent than in cold, such as copper(II) sulfate from its solution.

Section 6 of 11Simple distillation

Simple distillation
Use: separates a solvent from a solution, such as pure water from salt water, or a pure liquid from a mixture of liquids.
Method
  • Heat the solution, so the pure solvent evaporates and the vapour rises into the condenser.
  • The vapour cools and condenses to pure liquid, which is collected in a beaker.
  • The solid solute is left behind in the flask.
Simple distillation is less effective than fractional distillation when boiling points are close.

Section 7 of 11Fractional distillation

1
Use: separates two or more miscible liquids, such as ethanol and water, or the fractions of crude oil.
2
Principle: the liquid with the lowest boiling point evaporates first, is condensed and collected.
3
Ethanol boils at 78 °C and water at 100 °C, so stop heating when the temperature rises towards 100 °C.
4
Safety: an electric heater is safer than a flame with flammable liquids.
5
Crude oil is separated industrially, and it is not done in school because some components are toxic, but a synthetic crude oil can be used.
6
A gas mixture can be cooled until it liquefies and then separated by fractional distillation.
7
Diffusion can be used when boiling points are very close or distillation is impractical.

Section 8 of 11Choosing a separation method

MixtureMethod
Insoluble solid and liquidFiltration
Soluble solid from solutionCrystallisation or evaporation
Solvent from a solutionSimple distillation
Miscible liquids with different boiling pointsFractional distillation
Coloured soluble substancesPaper chromatography
Soluble and insoluble solidsDissolve, filter, then crystallise the filtrate

Section 9 of 11More from the specification

1Locating agents
  • Chemical substances sprayed onto a chromatogram to produce visible coloured spots from originally colourless components like amino acids.
2Distance moved (Rf value)
  • The ratio of the distance travelled by a solute spot relative to the distance travelled by the solvent front.
3Solubility separation (Calcium vs Magnesium)
  • Insoluble calcium sulfate is separated from soluble magnesium chloride by dissolving in water and filtering, then evaporating the filtrate.
4Crystallisation heating
  • A solution is gently heated until saturated crystals begin to produce along a glass rod, then left to cool.
5Chloride
  • Salt of hydrochloric acid.
6Locating agent
  • Chemical that makes colourless spots visible.

Section 10 of 11Key terms

TermMeaning
Filtratethe liquid or solution that passes through a filter.
Residuethe solid left on the filter paper.
Saturated solutiona solution holding the maximum solute at a given temperature.
Crystallisationforming crystals by cooling a saturated solution.
Simple distillationseparating a solvent from a solution by evaporating and condensing it.
Fractional distillationseparating miscible liquids by their different boiling points.
Pure substancea substance with sharp, specific melting and boiling points.

Section 11 of 11Exam technique

1
Saying the salt evaporatesthe water evaporates and the salt is left behind.
2
Mixing up filtrate and residuethe residue is the solid left on the paper.
3
Heating the crystallisation solution to dryness instead of removing no more than half.
4
Using simple distillation to separate miscible liquids with close boiling points.
5
Saying a pure substance melts over a range or that impurities raise the melting point: it has a sharp melting point and impurities lower it.

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