ATP
Paper 4
1 Experimental chemistry
Content
1.1 Experimental design
1.2 Methods of purification and analysis
1.3 Identification of ions and gases
It is expected that any course in chemistry will be based on experimental work.
Teachers are encouraged to develop appropriate practical work for candidates
to facilitate a greater understanding of the subject. Candidates should be
aware of the hazards and appropriate safety precautions to follow when
handling the reagents mentioned in this section.
learning outcomes
Candidates should be able to:
1.1 Experimental design
(a) Name appropriate apparatus for the measurement of time, temperature,
mass and volume, including burettes, pipettes, measuring cylinders and gas
syringes.
(b) Suggest suitable apparatus, given relevant information, for a variety of
simple experiments, including collection of gases and measurement of
rates of reaction.
1.2 Methods of purification and analysis
(a) Describe methods of purification by the use of a suitable solvent,
filtration and crystallization, distillation and fractional distillation, with
particular references to the fractional distillation of crude oil, liquid air and
fermented liquor.
(b) Suggest suitable methods of purification, given information about 0the
substances involved.
(c) Describe paper chromatography and interpret chromatograms including
comparison with ‘known’ samples and the use of Rf values.
(d) Explain the need to use locating agents in the chromatography of colourless
compounds.
(e) Deduce from the given melting point and boiling point the identities of
substances and their purity.
(f) Explain that the measurement of purity in substances used in
everyday life, e.g. foodstuffs and drugs, is important.
Measurement:
The following table shows the appropriate apparatus needed for the measurement of
time, temperature, mass and volume used in Experimental Chemistry.
Pipette: It is used to measure fix and accurate volume i.e. 10 cm3/25 cm3
Beaker:
It measures approximate volume:
Burette:
It measures the accurate volume of liquid
0.1cm3
i.e. 12.7, 20.3 etc.
Collection Of Gases:
Upward Delivery:
Upward delivery is used to collect gases that are less dense than air.
E.g. Hydrogen and Ammonia.
Downward Delivery:
Downward delivery is used to collect gases that are denser than air.
E.g. Chlorine and Hydrogen Chloride
Displacement Of Water:
Used for those gases which are insoluble in gases.
E.g. Hydrogen and Methane (CH4)
Collecting Dry Samples of Gases:
We can dry a gas by passing a drying agent through them as these agents will
absorb the moisture.
Drying Agents:
1 Concentrated Sulphuric Acid (H2SO4),
2 Quick Lime (Calcium Oxide (CaO)
3 Fused Calcium Chloride (CaCl2).
Concentrated Sulphuric Acid is used to dry moist gases like Chlorine and HCl.
However, it can’t be used to dry Ammonia because it reacts with Ammonia.
Techniques for Separation:
1. Filtration.
2. Crystallization.
3. Distillation.
4. Fractional Distillation.
5. Chromatography.
General Methods:
Method Use
Decanting It is used to separate a dense, insoluble solid from a
liquid.
Filtration It is used to separate insoluble solid from liquid.
The solid left behind is called residue.
The liquid which pass through filter paper is called
filtrate.
Evaporation to It is used when substance do not decompose on strong
Dryness heating.
Crystallization It is used to purify a substance which decompose on
strong heating.
Distillation To separate a liquid from solution.
Fractional To separate mixture of miscible liquids.
Distillation
1 Filtration:
It is used for separation of insoluble solid from a liquid.
Filtration is used to remove solid impurities from water/liquid.
Experiment:
• Place a filter paper into a filter funnel.
• Put the mixture of sand and water.
• The liquid will pass through as
• Sand as insoluble will remain on the filter paper as residue.
2 Crystallization:
It is an alternate method to recover a solute from its solution.
The solution is evaporating to the crystallization point i.e. two points at
which crystals of the solute will form on cooling, which can then be filtered
out and dried.
Experiment:
1. Solution is heated, the water evaporates and the solution becomes concentrated.
2. The saturated solution is then allowed to cool, crystals will start to form.
3. The saturated solution is cooled to form, crystals that can be dried on a
filter paper.
4. If evaporation needed, we will evaporate but not 100% since if evaporated
too much the crystals will convert themselves into powder.
Uses of Crystallization:
• Crystallization is used in obtaining pure sugar.
• Purification of antibiotics is used through crystallization.
Distillation:
Distillation is the method of obtaining a pure liquid (solute) from a solution of a solid
(solute).
Distillation Flask:
In this the solution boils, liquid vaporizes and enters the condenser.
Condenser:
In the condenser liquid vapour cools and it turns into pure liquid.
Experiment:
1. Water is allowed to flow through the condenser.
2. Solution in the flask is heated.
3. Collect the desired liquid (solvent) as distillate in the beaker until the
temperature starts to rise again.
Important steps to be taken during distillation:
1 The thermometer shouldn’t be dipped into the solution; this ensures that
the thermometer measures the boiling point of the substance that is being
distilled.
2 The condenser consists of two tubes. The cold running water is allowed to
enter the condenser from bottom and leave from the top.
3 The condenser slopes downwards, so that the pure solvent formed can run
into the beaker.
4 If the distillate is volatile, the receiver can be put in a large container
filled with ice.
Uses of Distillation:
• It is used to obtain pure water from sea water (desalination).
Fractional Distillation:
It is used to separate mixture of miscible liquids with different boiling points.
Fractionating Column: (B)
1 Fractionating Column is a column containing glass beads/glass wool in it
hence increasing the surface area, ensuring 100% separation and
purification.
2 The water vapour condenses in the fractionating column and drops back
into the flask, therefore insuring more purity.
3 The liquid with the lowest boiling will distill off first, as the fractionating
column will condense the liquids with higher boiling point and therefore it
will drop back into the flask.
4 The beaker can be changed after each liquid is distilled, to get other
liquids.
5 The thermometer will be used to identify which liquid is getting distilled
through its boiling point.
Uses of Fractional Distillation:
1 It is used in industries to obtain Nitrogen, Argon and Oxygen from Air.
2 It is used to separate crude oil into petrol, kerosene and other useful
components.
3 Fractional distillation is used to separate fermented liquor into ethanol and
water.
4 It is used to separate a mixture of miscible liquids.
Chromatography:
Chromatography is a process used to separate and identify two or more
substances from a mixture. Also, it is used to find out the number of
components in a liquid. Hence determining the purity of the substance.
Principles involved in chromatography:
• Each substance used, will have different solubility in the same solvent.
• If the substance is more soluble, it dissolves faster in the solvent. Hence
greater the solubility of the substance greater the distance it will be carried
away by the solvent, then that substance, which has less solubility.
A drop of the solution is placed on the origin line at the bottom of a chromatography
paper.
Rf Value
𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙 𝑏𝑦 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
𝑅𝑓 =
𝑇𝑜𝑡𝑎𝑙 𝑑𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑡𝑟𝑎𝑣𝑒𝑙 𝑏𝑦 𝑠𝑜𝑙𝑣𝑒𝑛𝑡
Separating and Identifying Mixtures of Colourless Substances
To do this a locating agent is to be sprayed on filter paper.
Locating Agent:
It is substance that reacts with substances (e.g. sugars) on Chromatogram to
produce a coloured product.
Uses:
1 To separate components in a sample.
2 Identify number of components.
3 Identify components present in sample.
4 Identify purity of a sample. (Pure sample have one spot).
Test for Aqueous Cations:
Effect of Aqueous sodium
Cations Effect of Aqueous Ammonia
hydroxide NaOH
white ppt., soluble in
Aluminum (𝑨𝒍 ) +𝟑
excess giving a white ppt., insoluble in excess
colourless solution
Ammonium ammonia produced on
(𝑵𝑯+𝟒 ) –
warming
Calcium (𝑪𝒂+𝟐 ) white ppt., insoluble in no ppt.
excess
green ppt., soluble in
Chromium (III)
excess, giving a green green ppt., insoluble in excess
(𝑪𝒓+𝟑 )
solution
light blue ppt., soluble in
Copper (II) light blue ppt., insoluble in
(𝑪𝒖+𝟐 ) excess excess, giving a dark
blue solution
Iron (II) (𝑭𝒆 ) +𝟐 green ppt., insoluble in green ppt., insoluble in excess
excess
Iron (III) (𝑭𝒆+𝟑) red-brown ppt., insoluble in red-brown ppt., insoluble in
excess excess
white ppt., soluble in white ppt., soluble in
Zinc (𝒁𝒏+𝟐) excess, giving a excess, giving a
colourless solution colourless solution
Test for Anions:
Anion Test Observation
Carbonate effervescence,
− add dilute acid carbon dioxide produced
𝑪𝑶𝟑 𝟐
Chloride (𝑪𝒍−𝟏 ) acidify with dilute nitric acid,
white ppt.
[in solution] then add aqueous silver nitrate
Iodide (𝑰−𝟏 ) acidify with dilute nitric acid,
yellow ppt.
[in solution] then add aqueous silver nitrate
Nitrate add aqueous sodium hydroxide, ammonia produced
−
𝑵𝑶𝟑 𝟏 then add aluminum foil; warm
carefully
[in solution]
−𝟐
Sulfate 𝑺𝑶𝟒 acidify with dilute nitric acid, white ppt., insoluble in excess
[in solution] then add aqueous barium dilute nitric acid
nitrate
Test for Gases:
Gas Test and test result
Ammonia (NH3) Turns damp red litmus paper blue
Carbon dioxide
Turns limewater milky
(CO2)
Chlorine (Cl2) Bleaches damp litmus paper
Hydrogen (H2) ‘Pops’ with a lighted splint
Oxygen (O2) Relights a glowing splint
It turns white anhydrous copper (II)
sulphate blue.
Water (H2O) It turns blue anhydrous cobalt (II) chloride
pink.
Titration:
Indicators: It shows the completion of reaction.
Indicator Colour in Acid Colour in base
Litmus Red Blue
Methyl Orange Red Yellow
Phenolphthalein Colourless Pink
Universal Red Violet
pH scale:
It is the scale to represents the strength of acid and alkali.
1 If 𝒑𝑯 > 𝟕 solution is alkaline.
2 If 𝒑𝑯 < 𝟕 solution is Acidic.
3 If 𝒑𝑯 = 𝟕 solution is Neutral.
Oxidizing Agent:
Oxidizing agent Observation
Acidified potassium dichromate (VI) Orange to green
Acidified potassium manganate (VII) Purple to colorless
Reducing Agent:
Reducing agent Observation
Aqueous Potassium iodide Color less to brown
Starch iodine paper color of moist starch paper change from
white to blue
Preparation of Salts:
Examples;
Method 1: (Starting substance is insoluble in water)
To prepare crystals by the reaction of acid with insoluble substance
(Metal):
(To prepare crystals of salts of Zn, Mg, Al, Fe less reactive metals.)
Crystals of soluble substance:
Steps:
1. Add excess dilute Sulphuric acid in a beaker then add metal and stir until
a gas is removed.
2. Filter the solution so separate filtrate.
3. Heat to concentrate.
4. Cool the filtrate to obtain the crystals.
5. Wash crystals with cold distilled water to remove impurities.
6. Dry the crystals between few sheets of dry filter paper.
To prepare crystals by the reaction of acid with base:
(To prepare Copper (II) sulphate crystal)
Crystals of soluble substance:
Steps:
1. Add excess dilute Sulphuric acid in a beaker then add 𝑪𝒖𝑶 until it is
saturated.
2. Filter the solution so separate filtrate.
3. Heat to concentrate.
4. Cool the filtrate to obtain the crystals.
5. Wash crystals with cold distilled water to remove impurities.
6. Dry the crystals between few sheets of dry filter paper.
To prepare crystals by the reaction of acid with Carbonates:
(To prepare Copper (II) sulphate crystal)
Crystals of soluble substance:
Steps:
1. Add excess dilute HCl in a beaker then add MgCO3 until no gas is
evolved.
2. Filter the solution so separate filtrate.
3. Heat to concentrate.
4. Cool the filtrate to obtain the crystals.
5. Wash crystals with cold distilled water to remove impurities.
6. Dry the crystals between few sheets of dry filter paper.
Method 2: (Starting material is soluble in water)
Titration:
(it is used to prepare crystals of Na, K and ammonium salts)
Crystals of soluble substance:
Steps:
1. Add 25cm3 base (NaOH) in a beaker, then titrate it by dilute HNO3. From
burette.
2. Heat the solution until it is concentrated.
3. Cool the solution to obtained crystals.
4. Filter to collect the crystals.
5. Dry the crystals between few sheets of dry filter paper.
Method 3: (Insoluble salts)
Precipitation:
Crystals of insoluble substance:
Steps:
1. Mix the two solutions and stir to formed precipitates.
2. Filter to collect precipitates.
3. Wash crystals with cold distilled water to remove impurities.
4. Dry the crystals between few sheets of dry filter paper.
