Topic 12 - Salt Preparation
Chapter 3 - Sec 3.3
A salt is the product of the reaction between an acid and a base.
Different techniques can be used to prepare different salts in the laboratory.
1. To prepare soluble salts 2. To prepare insoluble salts
A. Titration method C. Precipitation
B. Excess method:
1) Acid with excess metal technique
2) Acid with excess metal oxide technique
3) Acid with excess metal carbonate technique
A. Titration method:
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This method can be used when the salt to be formed and the base from which it is derived are both soluble.
This method is mainly used for the preparation of ammonium salts and alkali metal (group 1) salts.
Examples of questions from IGCSE Paper 3
Q1: Describe how crystals of ammonium sulphate can be made in the laboratory from aqueous ammonia.
Q2: Soluble salts such as sodium chloride are made by the reaction: base + acid → salt + water
Describe the preparation of sodium chloride from hydrochloric acid. Include in your account details
of any apparatus needed and name any other chemicals needed.
* Preparation of Sodium chloride crystals
* Steps:
1. Fill a burette till zero mark with aqueous sodium hydroxide.
2. Using a pipette, add 25 ml of the aqueous hydrochloric acid into a conical flask.
3. Add 2-3 drops of phenolphthalein indicator (in an acidic medium phenolphthalein is colourless).
4. Add aqueous sodium hydroxide to the hydrochloric acid solution, while continuously swirling, till the
end point is reached (point at which colour of the solution changes from colourless to permanent pale
pink upon adding a single drop of base).
5. Read the burette.
6. Repeat the experiment until you get concurrent results (readings that do not differ by more than 0.20
ml).
7. Take the average of three concurrent readings. This will be the average volume of the base needed to
neutralize the acid.
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8. Repeat the experiment one last time, by immediately adding the average volume of the base calculated
to the acid without using an indicator.
If it is required to prepare crystals of sodium chloride; this can be done by one of the following methods.
(a) Method 1
1. Heat the solution in an evaporating dish directly on a flame till most of the liquid evaporates.
2. Transfer the evaporating dish over a steam bath. Heat gently till all the liquid evaporates (do not
boil dry).
3. Leave to cool.
(b) Method 2:
1. Heat the solution in an evaporating dish directly on a flame till most of the liquid evaporates.
2. Transfer the evaporating dish over a steam bath. Heat gently till the crystallization point.
Crystallization point is checked by dipping a cold glass rod in the solution from time to time and
checking for the formation of crystals.
3. Leave to cool.
4. Filter off the crystals.
5. Dry the crystals between two filter papers without pressing.
• Related question that are asked:
Q: How can we tell that the neutralization point has been reached? [2]
Measure pH of the medium using a pH meter, pH will be 7 at neutralization point (as this is a
neutralization reaction)
• Notes:
1. To obtain dry crystals, dry residue between 2 filter papers without pressing.
2. To obtain powdered sample, dry the residue in an oven.
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B. Excess method:
General set up:
Typical Question
Describe how a solution of zinc sulphate could be made from the insoluble compounds of zinc
Several ways can be used to answer this question
Method I: Acid + Metal → Salt + Hydrogen
• Used for any metal that is more reactive than hydrogen (not suitable for the preparation of Cu or Ag
salts)
• Not suitable for the preparation of Na+, K+ salts as they are highly reactive metals and an explosion
could occur.
• Steps:
1. In a beaker, add a known volume of aqueous sulphuric acid.
2. Gently heat the acid in the beaker on a Bunsen burner (to speed up the rate of the reaction)
3. Turn off the burner. (To prevent splashing of the liquid).
4. Start adding spatula measures of the zinc metal to the acid and stir.
5. Continue adding the metal till:
a. Excess metal settles at the bottom of the beaker AND
b. No more bubbles of hydrogen gas evolve.
6. Filter. The residue is excess unreacted metal and the filtrate is zinc sulphate solution.
If crystals of zinc sulphate are required, this can be done by one of the crystallization techniques
discussed earlier.
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Method II: Acid + Metal Oxide → Salt + Water
• Used for any metal compound even Cu and Ag salts.
• Steps:
1. In a beaker, add a known volume of aqueous sulphuric acid.
2. Gently heat the acid in the beaker on a Bunsen burner (to speed up the rate of the reaction) throughout
the experiment.
3. Start adding spatula measures of zinc oxide to the acid and stir.
4. Continue adding the metal oxide till excess metal oxide settles at the bottom of the beaker.
5. Filter. The residue is excess unreacted metal oxide and the filtrate is zinc sulphate solution.
If crystals of zinc sulphate are required, this can be done by one of the crystallization techniques
discussed earlier.
Method III: Acid + Metal Carbonate → Salt + Water + Carbon dioxide
• Used for any metal compound even Cu and Ag salts.
• Steps:
1. In a beaker, add a known volume of aqueous sulphuric acid.
2. Start adding spatula measures of zinc carbonate to the acid and stir.
3. Continue adding the metal carbonate till:
a. Excess metal carbonate settles at the bottom of the beaker AND
b. No more effervescence is seen (due to evolution of CO2 gas).
4. Filter. The residue is excess unreacted metal carbonate and the filtrate is zinc sulphate solution.
If crystals of zinc sulphate are required, this can be done by one of the crystallization techniques
discussed earlier.
• Related question that may be asked:
Q: The volume of acid used in excess method is not specific .Explain
The solid (metal, metal oxide or metal carbonate) is added in excess to make sure that all the acid
has been used up (or reacted or consumed) irrespective of the volume of the acid used.
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• Summary:
Reagent Procedure How to know reaction is complete
(All acid has reacted)
Acid + Metal - Heat acid first. - Excess metal remains at the bottom of
- Put off Bunsen burner. the beaker
- Start adding spatula measures of - No more bubbles of hydrogen gas
metal. evolve.
Acid + Metal - Continue heating whilst adding the - Excess metal oxide remains at the
oxide metal oxide to the acid. bottom of the beaker.
Acid + Metal - No heating at all as effervescence - Excess metal carbonate remains at the
carbonate occurring is vigorous (to prevent bottom of the beaker
splashing of the liquid) - No more effervescence.
C. Precipitation method:
A typical, often asked question in Paper 3 of Cambridge IGCSE is of the form:
Q: How can a pure sample of the insoluble salt, lead (II) sulphate, be made?
• Steps:
Pb(NO3)2 (aq) + Na2SO4 (aq) → PbSO4 (s) + 2 NaNO3 (aq)
1. Add 25 cm3 , 1.0 M of aqueous sodium sulphate to 25 cm3 , 1.0 M of aqueous lead (II) nitrate in a
beaker.
➢ We must add equal number of moles of each reactant to make sure neither one remains in excess.
2. Stir with a glass rod.
3. Filter. The residue is lead(II) sulphate and the filtrate is sodium nitrate solution.
4. Wash the residue with distilled water to remove any impurities.
5. Dry the residue in an oven.
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