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Preparing a soluble salt by neutralisation

An acid and an alkali react to form a soluble salt in solution. Ammonia and sulfuric acid react to form ammonium sulfate, which can then be recovered by crystallisation.

Read our standard health & safety guidance

Lesson organisation

This is a well-tried standard class experiment, which should take no more than 30 minutes. If reagent solutions are provided in ready-measured quantities in small labelled bottles, the experimental work can start immediately.

Most classes should be able to perform this experiment as a class experiment but, if there are real doubts about safe behaviour or adequate manipulative skills while solutions are being heated, then student-aided demonstrations of these may be more sensible.

Apparatus and chemicals

Eye protection

Each working group requires:

Beaker (100 cm3)
Glass stirring rod (15 cm)
Evaporating basin (50–100 cm3 capacity)
Crystallising dish
Bunsen burner
Tripod
Heat resistant mat
Pipeclay triangle or gauze

Sulfuric acid, 0.5 mol dm-3 (Irritant at this concentration), 20 cm3 (in a small bottle)
Ammonia solution, 1 mol dm-3 (Low hazard at this concentration), 50 cm3 (in a small bottle)

Technical notes

Sulfuric acid (Irritant at concentration used) Refer to CLEAPSS Hazcard 98A and Recipe card 69
Ammonia solution (Low hazard at concentration used) Refer to CLEAPSS Hazcard 6 and Recipe card 4

Procedure

HEALTH & SAFETY: Wear eye protection

Stage 1

a Add 20 cm3 of 0.5 mol dm-3 sulfuric acid to the 100 cm3 beaker. Add 1 mol dm-3 ammonia solution slowly with stirring, about 5 cm3 at a time, until the solution smells faintly of ammonia even after stirring. (Students should be reminded how to smell chemicals safely.)

Stage 2

a Transfer the solution to an evaporating basin and place on a tripod with a pipeclay triangle or gauze.

b Heat the solution gently over a medium Bunsen flame so that water boils steadily.

c When about half the water has boiled away, take a drop of the hot solution on the end of a glass rod and let it cool. If the drop crystallises on cooling, the solution is ready for the next stage; if it does not crystallise, keep boiling and repeat the testing until the drop does crystallise on cooling. Do not boil dry.

Stage 3

a Pour the hot solution carefully into a crystallising dish.

b Set it aside to cool, with a label attached giving the name of the salt being prepared and the names of the group.

c Leave the crystallising dish in a warm place, safe from interference, until it has produced a good crop of crystals.

d If necessary, filter the solution, collect the crystals from the filter paper onto a paper towel, and allow to dry.

Teaching notes

There may be problems associated with younger students heating evaporating dishes perched on tripods, and with lifting hot apparatus off a hot tripod after heating. If there is any doubt about the safety of this step, you should lift each evaporating dish down onto the heat resistant mat first, before the students pour into the crystallising dish.

It is very important not to allow the students to boil the solution dry. If they do, the ammonium sulfate starts to decompose and release corrosive and toxic fumes into the laboratory.

The concentration of ammonia solution used is below that necessary for carrying a warning label. Nevertheless it is sensible to remind students to keep their faces away from the bottle of ammonia when it is open, and to replace the lid on the bottle whenever it is not in use.

The balanced equation for the reaction is only relevant for older students:

2NH3(aq) + H2SO4(aq) → (NH4)2SO4(aq)

Otherwise, a simple word equation is sufficient.
If a comparison with other acid-alkali neutralisations is made, then the equation in which ammonia solution is represented as NH4OH(aq) could be used, also showing water as one of the products of neutralisation:

2NH4OH(aq) + H2SO4(aq) → (NH4)2SO4(aq) + 2H2O(l)

Student questions

Stage 3

1 What substance do you think these crystals are? Give a reason for your answer.

2 Write word and symbol equations for the reaction you have done.

Health and safety checked, February 2008

Updated 29 Oct 2008

Average rating: 3 out of 5

Your reviews

This report is quiet detailed.
But, it's lost a step that's called recrystallisation?

Submitted by: Koh Kai Yung on 15 April 2009

Diagrams needed.

Submitted by: john on 28 April 2010

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