PRACTICAL TIPS

PROCEDURE
Reflux

Reflux for 30 min

Advantages of suction
filtration over normal filtration.
Aspects of the melting
temperature determination
that would indicate the crystals
were pure.
Adding drying agent

Adding anti-Bumping granules

Constant stirring

A solution is added drop wise

with cooling.
Washing with NaHCO3

REASON

RESULT

As liquid(s) vaporize, they

are cooled and condense back
to iquid(s)

Used to prevent the escape

of volatile substances and
thus increases the yield.
Reaction is slow / High activation
energy
Faster
Dries solid
Melting temperature
should besharp.
It should be consistent with
the literature.
To remove water
Eg:- Anhydrous MgSO4 or
Anhydrous Na2SO4 or Anhydrous
CaCl2
To ensure even boiling of liquids
Two possible answers
Reactants are immiscible
and they form separate
layers
To make sure that
temperature is uniform
throughout the solution
(Note: plan your answer
according to the situation)
Reaction is exothermic / To avoid
the temperature rising too much
Two possible answers
To neutralize excess acid
(when a pure sample is
prepared)
To quench the reaction
(when order of the reaction

Solution becomes clear

The pressure in the

funnel increases due to
the formation of CO2

to be found)
(Note: plan your answer
according to the
situation)
Precautions
1) Fume cupboard
2) Wear gloves

3) Water bath
Nitrous acid (HNO2) is made in
the reaction mixture rather than
being obtained from a chemical
supplier.
When Nitrous acid is used, the
temperature must not be lower
than 0C nor higher than 10C.
Recrystallization
1) Impure solid is dissolved
in a minimum volume of
hot solvent.
2) The solution is filtered
hot through a pre-heated
funnel.

3) The solution is cooled

and filtered using a
Buchner funnel.

i)
ii)

Toxic
Harmful by skin
absorption / corrosive
acid
iii)
Flammable liquid
HNO2 is unstable at room
temperature and hence, cannot be
stored.
Below 0oC, reaction is too slow
and above 10oC, diazonium
compound decomposes .
1) To prevent the solid
remaining in solution on
cooling.
2) To remove insoluble
impurities.
Pre-heated funnel is used
to prevent crystallization of
the solid.
3) Impurities remain soluble
and the pure solid
recrystallizes.

4) The solid is washed with

a small amount of cold
solvent.

4) To removes soluble
impurities.

5) The solid is dried in a

desiccator

5) To prevent decomposition.
Decomposition could occur
if the compound is
heated in an Oven.

Volume measurements
To measure 10-25cm3
solution, pipette is used.

An exact volume of
solution is needed.

More accurate

 Only an approximate
volume / excess is needed.

To measure more than

25cm3, measuring
cylinder is used.

It is incorrect to use HCl instead

of H2SO4 in KMnO4 titrations.

HCl will be oxidized to chlorine

by the manganate(VII)

Faster/More
convenient.

Titre value will be too

high.

I2 Vs Na2S2O3 titration

In burette - Na2S2O3
In pipette - I2 solution
Indicator Starch
Starch is added when the solution turns pale yellow.
Starch is not added initially because it forms an insoluble complex so that titre value
reduces and hence, the percentage error would be high(er).
When starch is added, solution becomes blue-black which turns colourless at the end
point.

Percentage yield.
Percentage yield =

Experimental value
Theoretical value

x 100%

Usually percentage yield is less than 100% because of,

i)
Transfer losses
ii)
Escape of volatile liquids
iii)
Impurities in the reactants
Sometimes, percentage yield is greater than 100% because The product is not dry / is damp.

Transfer losses
Solid (product) remains on the filter paper / is deposited on the sides of the glassware,
which is not be recovered by filtration.

Accuracy

Errors

Inorganic compounds and elements

1 Appearance

Coloured crystalline substances are usually hydrated salts of transition metals.

The colours of transition metal ions in dilute, aqueous solution are shown in the table
below.

2 Flame tests

To carry out a flame test, a clean nichrome wire is used to mix a sample of a solid with
one drop of concentrated hydrochloric acid. The wire is held in the hotter
Parts (blue) of a non-luminous Bunsen flame.

3 Heating
Gases or vapours may be evolved on heating a solid compound.

Action of dilute acids

When dilute sulfuric or hydrochloric acid is added to a substance a gas may be evolved
or there may be a colour change in the solution.

5 Recognition and identification of common gases

6 Hydrogen peroxide solution

Aqueous hydrogen peroxide (H2O2) can act as both an oxidizing and a reducing agent
often with the evolution of oxygen, although this may be unreliable.

7 Tests for oxidizing and reducing agents

PRECIPITATES
1 Barium chloride solution

NOTE:- If dilute hydrochloric acid is added to the anion solution before aqueous barium
chloride
then only the sulfate will form as a precipitate.

2 Sodium hydroxide solution

When dilute sodium hydroxide (NaOH) solution is added to a solution containing a
metal ion a precipitate of the insoluble hydroxide, eg Mn(OH)2, is usually formed.
Precipitates which are amphoteric hydroxides will dissolve in excess sodium hydroxide
to give a solution containing a complex ion, eg [Cr(OH)6]3.

3 Ammonia solution
Dilute aqueous ammonia (NH3), when added to a solution containing a cation, will
form the same hydroxide precipitate as dilute sodium hydroxide solution, eg Mn(OH) 2.
Excess aqueous ammonia may dissolve the precipitate to form a complex ion,
eg [Cu(NH3)4(H2O)2]2+.

4 Silver nitrate solution

Aqueous silver nitrate is commonly used to test for the presence of halide ions in
solution. Anions which would interfere with the test (eg carbonate) are removed by
adding dilute nitric acid before the aqueous silver nitrate.
Silver halides which dissolve in ammonia do so to form a colourless solution of the
complex ion, [Ag(NH3)2]+.

5 Concentrated sulfuric acid

When a few drops of concentrated sulfuric acid (H2SO4) are added to a solid halide the
observed reaction products may be used to identify the particular halide ion present.
This is a potentially hazardous reaction.
It must be carried out on a small scale and in a fume cupboard.

 The products in brackets will not be observed since they are colourless gases.

ORGANIC COMPOUNDS
1 Solubility

2 Chemical tests

3 Ignition

Organic reactions

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