Unit 3

Practical Written Examination

At both AS and A2 Level Practical skills being assessed in the
examinations are:
 Qualitative observation
 Quantitative measurments
 Preparation

Qualitative observation
This includes the instruction of each test to be carried out usually on a test tube
scale. By learning about these test students are able to identify any unknown salt or
organic compound. Similarly unknowns will be limited to compounds containing
the ions, elements and organic compounds with the functional groups listed for the
specification. To identify an unknown organic compound, spectroscopic data may
be included for students to analyse.

Quantitative measurements
In this part the examination could involve information on the use of apparatus to
make measurements and to process the results, to draw graphs, conclusions. This
type of questions could involve
 A volumetric analysis
 Simple thermo chemistry
 Rate of a reaction
Preparation
This part include questions in which a procedure has been followed to prepare and
in some cases purification of compound. Purification can include some of the
following laboratory procedures.
 Simple distillation
 Heat under reflux
 Filtration
 Purification by washing in a separating funnel
 Solvent extraction
 Drying
In some preparation questions students may be asked to calculate the maximum
mass of product and a percentage yield

Inorganic substances

You may assume only the following ions and gases will be tested.

Cation Li+ Na+ K+ Mg2+ Ca2+ Sr2+ Ba2+ NH4+

Anion Cl- Br- I- NO3- CO32- HCO3- SO42- SO32-

Gases H2 O2 Cl2 CO2 NH3 SO2 HCl

Test for cations
How to carry out the flame test
Flame test
Make sure that the wire is clean by dipping it into some concentrated hydrochloric acid and then
putting it into the hot part of the bunsen flame. Repeat until the flame is not coloured. Now dip
the wire into conc hydrochloric acid and then into the solid and immediately place it in the
hottest part of the Bunsen flame

The following flame colours are observed

Strontium ion Crimson

Barium ion Apple green

Scarlet red
 NH4+

Test for anions

Test for halide ions

AgNO3(aq)+ NaCl(aq)  AgCl (s) + NaNO3(aq)

White ppt

AgNO3(aq)+ NaBr(aq)  AgBr (s) + NaNO3(aq)

cream

AgNO3(aq)+ NaI(aq)  AgI(s) + NaNO3(aq)

yellow

How do you confirm the presence of these ions

Slightly soluble
 Test for carbonate (CO32-) and hydrogen carbonate ions (HCO3-)

Chemical test Add any dilute strong acid to the suspected solid
for Carbonate ion CO32– or carbonate
hydrogencarbonate if colourless gas given off, test with limewater.
HCO3– ion
(Effect of fairly strong heating and testing for any carbon
dioxide

given off.

Test (ii) will distinguish sodium hydrogencarbonate

(NaHCO3 readily decomposes – 'baking powder') from

anhydrous sodium carbonate (Na2CO3, thermally very

Acid is added to the solid stable).
carbonate in a test tube. You
could also collect a sample
of gas from a heated
carbonate, i.e. the solid is
where the liquid is in the left
hand test tube.

Methods of gas
preparation are described in
more detail on another page.

(i) Fizzing – colourless gas which turns limewater milky – cloudy fine white
precipitate (see above CO2).

(ii) There might be colour changes in the solid, but you need to collect a sample of gas
from just above the heated solid to see it gives a white precipitate with limewater.

Apart from hydrated sodium carbonate, sodium hydrogencarbonate is one of the few
common carbonates to give off water on heating and condenses on side of test tube,
but basic carbonates will also give off H2O as well as CO2.

(i) To identify any carbonate/hydrogencarbonate + acid  salt + water + carbon

dioxide, then white precipitate with limewater. The ionic equations are for carbonate ...

CO32–(s) + 2H+(aq) H2O(l) + CO2(g)

and for the hydrogencarbonate ...

HCO3–(s) + H+(aq)  H2O(l) + CO2(g)

(ii) The thermal decomposition equations are for carbonates

MCO3(s) MO(s) + CO2(g)

e.g. M = Mg, Zn, Cu and note that some give clear colour changes in the solid
which might be useful to identify the metal (see heating carbonates in metal
cation section) CuCO3 CuO + CO2

green solid black

and for sodium hydrogencarbonate ...

2NaHCO3(s) . Na2CO3(s) + H2O(l) + CO2(g)

Na2CO3  Do not decompose on heating

Test for sulphate ions

Sulphate ion or sulphate(VI) ion Test

SO42– [sulfate, sulfate(VI)] chemical test To a solution of the suspected sulfate add dilute
hydrochloric and a few drops of
IfTest for Sulphate
the solution ions:
also contains the chloride barium chloride/ nitrate solution.
ion, you test with barium ions 1st, filter
off any bariumSOsulphate
2- precipitate and
4
then test for chloride ion. This is
because silver sulphate is also
~insoluble.(ppt)

Observation Chemistry involved

A white precipitate of barium sulfate. Ba2+(aq) + SO42–(aq) . BaSO4(s)
Any soluble barium salt + any soluble sulphate forms

a white dense barium sulphate precipitate.

 Sulphite ion or sulphate(IV) ion Test
SO32– [sulfite, sulfate(IV)] chemical test (i) Add dilute hydrochloric acid to the suspected sulfite.
Test for Sulphite Ions
Test (iii) is easily unreliable, the sulphite (ii) Test any gas evolved with fresh
ion is oxidised 2-by air (dissolved oxygen)
SO
to give the sulphate ion, so you will
3 potassium dichromate(VI) paper.K2Cr2O7
lucky to obtain a clear solution after
adding excess acid. (iii) Add barium chloride or barium nitrate solution
Chemistry involved
Observation
Acrid choking sulfur dioxide gas (i) To identify any sulphite salt + hydrochloric acid
formed. chloride salt + sulphur dioxide.+ water

(ii) The dichromate paper turns (ii) The sulphur dioxide reduces the dichromate(VI)
from orange to green.
to chromium(III). Note: sulphites do not give ppt.
(iii) A white ppt. of barium sulphite
which dissolves in excess with acidified barium chloride/nitrate because sulphites
hydrochloric acid to give a clear
colourless solution. dissolve in acids.

(iii) Ba2+(aq) + SO32–(aq)  BaSO3(s)

BaSO3(s) + 2HCl(aq) . BaCl2(aq) + H2O(l) + SO2(aq)

Test 1
A 1 Add dil hydrochloric acid to both
B 2 Then add few drop s of BaCl2solution
Observation
Test tube B gives a white ppt. but no ppt in A
Conclusion;
Test tube B has sulphate salt and test tube A
has sulphite salt

Sulphate salt solution

Sulphite salt
solution Test 2
1 Add BaCl2 to both
2 Then add dil HCl to both
Observation
1 tube A and B produce white ppt
2 tube A ppt dissolves reacting it with acid, but tube B ppt
remain unchange
Nitrate ion or nitrate(V) ion Test
NO3– chemical test Boil the suspected nitrate with sodium hydroxide solution
Test for nitrate ions and fine aluminium powder (Devarda's Alloy) or aluminium foil.

Then hold a damp red litmus paper to the mouth of the test tube

Observation (i) The aluminium powder is a powerful reducing agent and converts the n
the fumes contain ammonia, which ammonia gas, NH3
turns red litmus blue,
.

Test for gases

Test for
ammonia
 Bubble the gas Colour changes
through acidified from orange to
potassium dichromate green
solution

The action of concentrated sulfuric acid on sodium halides

Sodium halides (NaCl, NaBr and NaI only) with concentrated sulfuric acid

Sodium chloride

When concentrated sulfuric acid is added to sodium chloride,

 white misty fumes of hydrogen chloride are observed.

 NaCl(s) + H2SO4 (l) NaHSO4 (s)+ HCl(g) *

 Hydrogen chloride gas is not a strong enough reducing agent to affect

the concentrated sulfuric acid. (TEST for HCl gas : bring a bottle cap
of conc. ammonia closer to HCl gas. It produces thick white smoke)
  Steamy fumes of hydrogen chloride gas is observed
 Produces a white smoke (ammoniumchloride) with ammonia gas

Sodium bromide

When concentrated sulfuric acid is added to sodium bromide,

 white misty fumes of hydrogen bromide are observed together with

brown fumes of bromine.

 The reason is that hydrogen bromide is a strong enough reducing

agent to react with concentrated sulfuric acid.

 NaBr(s) + H2SO4(l) NaHSO4(s) + HBr(g) *

 H2SO4(l)+ 2HBr(g) Br2+ SO2+ 2H2O *

 Hydrogen bromide reduces sulfur from oxidation state +6 in H2SO4 to

+4 in SO2.

Sodium iodide

When concentrated sulfuric acid is added to sodium iodide,

 on warming purple fumes of iodine are observed together with the
smell of hydrogen sulfide.(rotten egg)

 NaI(s) + H2SO4(l) NaHSO4+ HI *

 H2SO4+ 8HI 4I 2+ H2S + 4H2O *

 Hydrogen iodide is the strongest reducing agent of the three

hydrogen halides and reduces sulfur from +6 in H2SO4to-2 in H2S.

Summary:
 When a few drops of conc.sulphuric acid 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. The halide ion may be identified without the need to
test for these gases. No attempt should ever be made to detect these
gases by smell.


Halide Observations on adding conc Observed reaction
H2SO4 products
Chloride Steamy fumes, vigorous HCl(g)
reaction
Bromide Steamy fumes, brown vapour, HBr(g),Br2(g), (SO2)
Vigorous reaction
Iodide Steamy fumes, black solid, I2, S ,(H2S)
purple vapour, yellow solid,
vigorous reaction