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Chemistry · Practical skills

Experimental techniques & chemical analysis

CIE 06203 min read

Experimental design

Apparatus:

  • Stopwatches — measuring time
  • Thermometers — measuring temperature
  • Balances — measuring mass
  • Burettes — measuring liquid volume
  • Volumetric pipettes — measuring a fixed volume of liquid
  • Measuring cylinders — measuring liquid volume
  • Gas syringe — measuring gas volume

Key terms:

  • Solvent — dissolves a solute
  • Solute — the substance getting dissolved
  • Saturated solution — solution with the maximum concentration of dissolved solute at a temperature
  • Residue — the substance left after filtration of a solution
  • Filtrate — the substance produced after successfully passing through the filter

Acid–base titrations

Titration is the neutralisation of a soluble base (potassium, ammonium and sodium hydroxides) and acid.

Equipment:

  • Burette
  • Volumetric pipette
  • Indicator

Method:

  1. Fill a burette with acid
  2. Fill a conical flask with a known volume of an alkali (using volumetric pipette)
  3. Add a few drops of indicator into the alkali (e.g. thymolphthalein)
  4. Drop the acid from the burette into the alkali, swirling the solution as you go
  5. Stop when the colour of the indicator changes (it has reached its end-point)
  6. Record the volume of acid used
  7. Repeat the experiment without the indicator, using the known volume of acid

Chromatography

Chromatography is used to separate soluble inks and smaller molecules (e.g. amino acids).

Rf value equation:

Rf = Distance travelled by substance / Distance travelled by solvent

Rf value < 1

  • If chromatography is used to separate colourless substances, a locating agent is required to identify where the substance has travelled to

Separation and purification

Methods:

  • Filtration
  • Crystallisation
  • Simple distillation
  • Fractional distillation

Distillation is a separation technique that takes advantage of the different boiling points of substances.

If the wanted substance is insoluble

  • Filter
  • Wash the residue
  • Dry the residue in an oven

If the wanted substance is soluble

  • Filter
  • Crystallise the filtrate

Separation of 2 liquids

  • Simple distillation

Separation of liquids with similar boiling points

  • Fractional distillation
  • Uses a fractionating column to separate the liquids

Identification of ions and gases

Anion tests

AnionTestResult
CarbonateReact with dilute acid then test for carbon dioxide using limewaterBubbling and limewater turns cloudy/milky
ChlorideAcidify with dilute nitric acid and add aqueous silver nitrateWhite precipitate forms
BromideAcidify with dilute nitric acid and add aqueous silver nitrateCream precipitate forms
IodideAcidify with dilute nitric acid and add aqueous silver nitrateYellow precipitate forms
NitrateAdd aqueous sodium hydroxide and then aluminium foil. Warm the mixture.Bubbling, gas produced that turns damp red litmus paper blue (ammonia)
SulfateAcidify with dilute nitric acid and add aqueous barium nitrateWhite precipitate formed
SulfiteAdd acidified aqueous potassium manganate(VII)The potassium manganate(VII) changes from purple to colourless

Cation tests

CationAqueous sodium hydroxideAqueous ammonia
AluminiumWhite precipitate formed, soluble in excess forming a colourless solutionWhite precipitate formed, insoluble in excess
AmmoniumOn warming, a gas is produced that turns damp red litmus paper blue (ammonia)No reaction
CalciumWhite precipitate formed, insoluble in excessNo precipitate / very little white precipitate
Chromium(III)Green precipitate formed, soluble in excessGreen precipitate, insoluble in excess
Copper(II)Light blue precipitate formed, insoluble in excessLight blue precipitate, soluble in excess forming a dark blue solution
Iron(II)Green precipitate formed, insoluble in excessGreen precipitate formed, insoluble in excess
Iron(III)Red-brown precipitate formed, insoluble in excessRed-brown precipitate formed, insoluble in excess
ZincWhite precipitate formed, soluble in excess forming a colourless solutionWhite precipitate formed, soluble in excess forming a colourless solution

Test for gases

GasTestResult
AmmoniaDamp red litmus paperTurns blue
Carbon dioxideLimewaterTurns milky
ChlorineDamp litmus paperBleaches
HydrogenLighted splintGoes off with a squeaky pop
OxygenGlowing splintRelights
Sulphur dioxideBubble through acidified potassium manganate(VII)Changes from purple to colourless

Flame test to identify cations

Using a nichrome wire loop, dip it into some HCl and hold it to the flame, this cleans the loop. Dip the loop into the cation sample and hold it to a blue flame. Observe the colour changes.

CationFlame colour
LithiumRed flame
SodiumYellow flame
PotassiumLilac flame
CalciumOrange-red flame
BariumYellow-green flame
CopperBlue-green flame

Test yourself

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