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Cambridge IGCSE Chemistry (0620) · Topic 12 — Experimental techniques and chemical analysis
Mini-Lesson

Experimental techniques & chemical analysis

This mini-lesson covers the whole of Cambridge IGCSE Chemistry (0620) Topic 12: measurement, acid–base titrations, criteria of purity, paper chromatography & Rf, methods of purification, and the identification of ions and gases.

Extended only: the lilac Supplement pill marks statements assessed only on the Supplement (extended) papers. Everything else is Core and Supplement.

unknown mixture separate pure substance test identify ions/gases

Work through each screen, answer the questions as you go (some are wordy, some are calculations) and collect ⭐ stars. Press Start when you're ready.

12.1 Measurement

Choosing apparatus to measure

Good chemistry starts with the right tool for the quantity you are measuring:

  • Time — a stopwatch/clock (in seconds).
  • Temperature — a thermometer (in °C).
  • Mass — an electronic balance (in g).
  • Volume of a liquid — choose by the precision you need.
  • Volume of a gas — a gas syringe (or collection over water).
measuring cylinder pipette burette gas syringe
For an exact, accurate volume use a pipette or burette; a measuring cylinder is quick but rough. Gas volume → gas syringe.

Watch out: a measuring cylinder reads to ~±1 cm³ — fine for "about 25 cm³", but for a titration you need the precision of a pipette (fixed volume) and a burette (variable, read to 0.05 cm³). Always read the bottom of the meniscus at eye level.

Quick check

Pick the apparatus

?You must add exactly 25.0 cm³ of acid to a flask, and the volume must be accurate. Which piece of apparatus is best?
12.1 Acid–base titrations

Carrying out a titration

A titration finds the exact volume of one solution that reacts with another. The method:

  • Pipette a fixed volume of one solution (e.g. 25.0 cm³ of alkali) into a conical flask.
  • Add a few drops of a suitable indicator.
  • Burette in the acid, swirling, until the indicator just changes colour — the end-point.
  • Record the burette readings and repeat for concordant (close-agreeing) results.
acid in burette tap controls flow alkali + indicator white tile (see colour) Read the meniscus eye level, bottom of curve Suitable indicators litmusred ⇄ blue thymolphthaleincolourless ⇄ blue methyl orangered ⇄ yellow
The burette (acid) sits above a conical flask (alkali + indicator) on a white tile. Add acid until the indicator just changes — the end-point.

Suitable indicators: the 0620 syllabus names litmus, thymolphthalein and methyl orange. (A universal indicator is not used for titrations — its gradual colour change gives no sharp end-point.)

Quick check

Why not universal indicator?

?In an acid–base titration, why is thymolphthalein or methyl orange used instead of universal indicator?
12.2 Criteria of purity

Melting & boiling points test purity

A pure substance melts and boils at fixed, sharp temperatures. An impurity:

  • lowers the melting point and makes it melt over a range (not sharp);
  • raises the boiling point and makes it boil over a range.
temperature → pure: sharp m.p. impure: melts over a range (and at a lower temperature)
Comparing a measured m.p./b.p. with the known value for the pure substance tells you whether — and roughly how — it is impure.

Watch out: melting and boiling points are used to test purity — they are not a way to purify anything. A truly pure substance has a sharp, single melting point; a range means impurity.

Quick check

Reading a melting point

?Pure aspirin melts sharply at 135 °C. A student's sample melts over the range 128–132 °C. What does this tell you?
12.2 Paper chromatography

Separating with chromatography

Paper chromatography separates a mixture of soluble, coloured substances (e.g. inks, food dyes):

  • Draw a baseline in pencil (pencil doesn't dissolve in the solvent).
  • Spot the mixture on the baseline; dip the paper in solvent below the baseline.
  • The solvent rises, carrying each substance a different distance.
  • The solvent front and the spots move; the most soluble travels furthest.
solvent front baseline (pencil) d(spot) = 4.8 cm d(solvent) = 6.0 cm measure to spot centre solvent level starts below the baseline
Measure each distance from the baseline to the centre of the spot, and from the baseline to the solvent front.

Watch out: the baseline must be pencil (ink would dissolve and run), the solvent must start below the baseline (or the spots wash off), and distances are measured to the centre of each spot.

12.2 Rf values

Calculating an Rf value

To compare chromatograms we calculate each spot's Rf value — a ratio that is the same for a given substance and solvent:

Rf = distance moved by substance ÷ distance moved by solventboth distances measured from the pencil baseline; the spot distance is taken to the centre of the spot
Worked example

A spot moves 4.8 cm from the baseline; the solvent front moves 6.0 cm.

Rf = 4.8 ÷ 6.0 = 0.80 (no units)

Watch out: Rf has no units and is always less than 1 (the spot can never travel further than the solvent). Matching Rf values against known substances identifies an unknown.

Calculate

Your turn — Rf value

1On a chromatogram a dye travels 3.6 cm from the baseline while the solvent front travels 4.5 cm. Calculate the Rf value of the dye.
(no units)
Hint: Rf = 3.6 ÷ 4.5. The answer must be less than 1.
12.2 Chromatography Supplement

Locating agents & two-way chromatograms

Many substances — such as amino acids and sugars — are colourless, so their spots are invisible. A locating agent is sprayed on to make them show up.

  • e.g. ninhydrin reacts with amino acids to give coloured (purple) spots so their positions can be seen and Rf values found.

Two-way chromatography separates substances that have similar Rf values in one solvent:

  • Run the chromatogram in one solvent, then turn the paper 90° and run it again in a different solvent.
  • Spots that overlapped in the first run are pulled apart in the second.
origin solvent 1 solvent 2 (turn 90°) Overlapping spots from solvent 1 are pulled apart by solvent 2.
Supplement A two-way chromatogram: a second solvent at 90° resolves spots that had the same Rf in the first.
Quick check Supplement

Seeing colourless spots

?A mixture of colourless amino acids is run on chromatography paper. Why is a locating agent (e.g. ninhydrin) needed?
12.3 Methods of purification

Choosing a separation method

You must match the method to the mixture:

MethodSeparates…
Filtrationan insoluble solid from a liquid (e.g. sand from water)
Crystallisationa dissolved solid from its solution (e.g. salt from salt solution), by evaporating to a hot saturated solution, then cooling so crystals form
Simple distillationa solvent from a solution (e.g. pure water from salt water)
Fractional distillationtwo or more miscible liquids with different boiling points (e.g. ethanol from water)
residue (insoluble solid) stays on the filter paper filtrate (the liquid) passes through into the beaker
Filtration: the residue (insoluble solid) stays on the paper; the filtrate (liquid) passes through.

Watch out: to get the solid back from a solution you crystallise (don't boil dry — that decomposes hydrated crystals). To get the solvent back you distil. Use fractional distillation only when the liquids both evaporate (similar, but different, boiling points).

Match it

Which method?

Tap a mixture on the left, then tap the method on the right that separates it.

12.4 Identification of cations · flame tests

Flame tests for metal cations

Hold a sample on a clean wire in a hot, blue Bunsen flame. The metal cation gives a characteristic flame colour:

Li⁺red Na⁺yellow K⁺lilac Cu²⁺blue-green Ca²⁺orange-red
Flame colours: Li⁺ red · Na⁺ yellow · K⁺ lilac · Cu²⁺ blue-green · Ca²⁺ orange-red.

Watch out: sodium's strong yellow easily masks other colours, so the wire must be clean (dip in acid first). Flame colour identifies the metal ion only.

Quick check

Name that flame

?A salt gives a lilac flame in a flame test. Which cation is present?
12.4 Cations · NaOH & aqueous NH₃

Testing cations in solution

Add a few drops, then excess, of aqueous sodium hydroxide or aqueous ammonia. Note the colour of the precipitate and whether it dissolves in excess:

Cationwith NaOH(aq)with NH₃(aq)
NH₄⁺no ppt; on warming gives ammonia gas (red litmus → blue)
Cu²⁺light blue ppt, insoluble in excesslight blue ppt, dissolves in excess to give a dark blue solution Supplement
Fe²⁺green ppt, insoluble in excessgreen ppt, insoluble in excess
Fe³⁺red-brown ppt, insoluble in excessred-brown ppt, insoluble in excess
Ca²⁺white ppt, insoluble in excessno ppt (or very slight)
Zn²⁺ Supplementwhite ppt, dissolves in excess (colourless)white ppt, dissolves in excess (colourless)
Al³⁺ Supplementwhite ppt, dissolves in excess (colourless)white ppt, insoluble in excess

Watch out: Zn²⁺ and Al³⁺ both give a white ppt that dissolves in excess NaOH — tell them apart with ammonia: Al³⁺'s ppt stays, Zn²⁺'s redissolves. Supplement The Cu²⁺ ppt redissolving in excess ammonia to a deep blue is a Supplement detail.

Identify the ion

Reading the results

?An unknown solution gives a red-brown precipitate with sodium hydroxide that does not dissolve in excess. Which cation is present?
12.4 Identification of anions

Testing for anions

AnionTestPositive result
Carbonate CO₃²⁻add dilute acidfizzes; CO₂ given off (turns limewater milky)
Chloride Cl⁻acidify with dilute nitric acid, add silver nitratewhite precipitate (AgCl)
Sulfate SO₄²⁻acidify with dilute nitric acid, add barium nitratewhite precipitate (BaSO₄)
Nitrate NO₃⁻ Supplementadd aqueous NaOH then aluminium foil, warmammonia gas given off (red litmus → blue)
Sulfite SO₃²⁻ Supplementadd dilute acid and warm (or acidified potassium manganate(VII))SO₂ given off; turns acidified KMnO₄ from purple to colourless

Watch out: always acidify first with dilute nitric acid before the chloride/sulfate tests — this removes carbonate ions, which would also give a precipitate and mislead you. Supplement The nitrate and sulfite tests are Supplement (extended) only.

Identify the ion

Which anion?

?A solution is acidified with dilute nitric acid, then silver nitrate is added. A white precipitate forms. Which anion is present?
12.4 Identification of gases

Testing for gases

GasTest & positive result
Ammonia NH₃turns damp red litmus paper blue
Carbon dioxide CO₂turns limewater milky (cloudy white)
Chlorine Cl₂bleaches damp litmus paper (turns it white)
Hydrogen H₂lighted splint → "squeaky pop"
Oxygen O₂relights a glowing splint
Sulfur dioxide SO₂ Supplementturns acidified aqueous potassium manganate(VII) from purple to colourless

Watch out: a lighted splint (pop) tests for hydrogen; a glowing splint (relights) tests for oxygen — don't mix them up. Supplement The sulfur dioxide test is Supplement (extended) only.

Match it

Match the gas to its test

Tap a gas on the left, then tap its correct test result on the right.

Recap

Topic 12 — the essentials

Measurement: pipette/burette = accurate volume; gas syringe = gas volume; balance = mass.

Titration: pipette + burette + a single indicator (litmus, thymolphthalein, methyl orange) → sharp end-point.

Purity: a pure substance has a sharp m.p./b.p.; impurity lowers & broadens m.p., raises b.p.

Chromatography: pencil baseline, measure to spot centre; Rf = substance ÷ solvent (no units, < 1).

Supplement: locating agents, two-way chromatograms.

Purification: filtration · crystallisation · simple & fractional distillation — match to the mixture.

Identifying ions: flame colours; NaOH/NH₃ precipitates (cations); acid + AgNO₃/Ba(NO₃)₂ (anions).

Identifying gases: NH₃, CO₂, Cl₂, H₂, O₂ (+ SO₂ Supplement).

You've covered all of Cambridge IGCSE Chemistry (0620) Topic 12. Press Finish to see your score.

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