PRACTICAL TIPS

PROCEDURE REASON RESULT

Reflux 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.

Reflux for 30 min Reaction is slow / High activation
energy

Advantages of suction
filtration over normal filtration.
Faster
Dries solid

Aspects of the melting
temperature determination
that would indicate the crystals
were pure.
Melting temperature
should besharp.
It should be consistent with
the literature.

Adding drying agent To remove water
Eg:- Anhydrous MgSO
4
or
Anhydrous Na
2
SO
4
or Anhydrous
CaCl
2

Solution becomes clear
Adding anti-Bumping granules To ensure even boiling of liquids
Constant stirring 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)

A solution is added drop wise
with cooling.
Reaction is exothermic / To avoid
the temperature rising too much

Washing with NaHCO
3
Two possible answers
To neutralize excess acid
(when a pure sample is
prepared)

To quench the reaction
(when order of the reaction
to be found)
(Note: plan your answer
according to the
situation)

The pressure in the
funnel increases due to
the formation of CO
2


Precautions
1) Fume cupboard
2) Wear gloves


3) Water bath

i) Toxic
ii) Harmful by skin
absorption / corrosive
acid
iii) Flammable liquid

Nitrous acid (HNO
2
) is made in
the reaction mixture rather than
being obtained from a chemical
supplier.
HNO
2
is unstable at room
temperature and hence, cannot be
stored.

When Nitrous acid is used, the
temperature must not be lower
than 0C nor higher than 10C.
Below 0
o
C, reaction is too slow
and above 10
o
C, diazonium
compound decomposes .

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.

4) The solid is washed with
a small amount of cold
solvent.

5) The solid is dried in a
desiccator


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) To removes soluble
impurities.


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

Volume measurements
To measure 10-25cm
3

solution, pipette is used.

To measure more than
25cm
3
, measuring
cylinder is used.


An exact volume of
solution is needed.

Only an approximate
volume / excess is needed.

More accurate


Faster/More
convenient.

It is incorrect to use HCl instead
of H
2
SO
4
in KMnO
4
titrations.

HCl will be oxidized to chlorine
by the manganate(VII)

Titre value will be too
high.


I
2
Vs Na
2
S
2
O
3
titration
In burette - Na
2
S
2
O
3
In pipette - I
2
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 =


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.




4 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(NH
3
)
4
(H
2
O)
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(NH
3
)
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



















Phenol