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Qualitative Analysis Guide Sheet for C.S.E.E. Chemistry Practical

Systematic Qualitative Analysis can be grouped into three stages:
1) Preliminary tests
2) Tests in solution
3) Confirmation tests
The ions expected in the scheme include:
Cations: NH4+ Ca2+ Fe3+ Cu2+ Zn2+ Pb2+ Na+ Fe2+
Anions: CO32- HCO3- NO3- SO42- ClRecording experimental results
The recorded results should appear in a tabular form where three columns showing the brief explanation of the
experimental procedure, observations made, and inferences must appear.
The report should be in the following table:
TEST

OBSERVATIONS

INFERENCE

OBSERVATIONS:
When doing experiments, leave the chemicals to stand for a few minutes as some changes may take a little time to be
seen. For example, most precipitates form instantly, but others take a minute or two.
Thus observations are generally changes which can be seen when a chemical substance is subjected to an experiment
(test). These include:
a) colour change
b) precipitates formed
c) gelatinous changes of liquid substances
d) gases evolved
e) light (noise) produced
INFERENCE:
Inferences are essential in experimental procedure as they explain about the identity of the unknown chemical
substances. Usually inferences must be specific. For example a common mistake of making deductions is to write
sodium, Na+ . Does this mean sodium Na+ ions are present or absent? Students should remember to write specific
inferences. Students should also remember that not all experiments will give a visible change. Sometimes if there is no
change, it can help to make an inference about the absence of certain ions. For example, if a barium nitrate solution
added to an unknown substance and there is no reaction, this implies that sulphate ions are absent because the
presence of sulphate ions is shown by formation of white precipitate.
CONCLUSION:
Before proceeding to the next test, observations and inferences of the earlier experiment must be written. After all
experiments you may be asked to make conclusions about the chemical ions or nature of the chemical substances
found in the samples. This can be obtained by combining together all inferences made earlier in the successive tests.

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1) Preliminary Tests
Preliminary tests of a sample involve:
i)
Appearance: form, colour, smell, and acidity
ii)
Solubility of a substance in water
iii)
Action of heat on a solid sample
iv)
Action of dilute H2SO4 on a solid sample
v)
Action of concentrated H2SO4 on a solid sample
vi)
Flame test
PRELIMINARY TESTS:
TEST

OBSERVATIONS
White crystalline substance

Blue/Green crystals
Light green, turning almost colourless
when dissolved in water
Yellow/golden yellow
Gives smell of ammonia
Colourless liquid forming droplets on
the cooler part of the test tube. Liquid
turns anhydrous CuSO4 blue
White sublimate and ammonia gas
detected
Residue yellow when hot and white
when cold
Residue reddish brown when hot yellow
Action of heat on a solid sample (put when cold
a little solid sample in a clean and dry Brown gas which turns litmus paper red
tests tube and heat it)
NO2 evolved
Colourless gas which turns potassium
dichromate green SO2 gas evolved
Colourless gas which turns lime water
milky CO2 gas evolved
Green or blue salt turns black and
remain as black residue
Reddish brown residue; dark coloured
when hot
Action of dilute Sulphuric acid
Effervescence and a gas evolved turns
(H2SO4) on the sample
lime water milky - CO2 evolved
Colourless gas which gives white fumes
with ammonia HCl evolved
Brown fumes which intensifies on
addition if copper turnings NO2 is
Action of concentrated Sulphuric
acid (H2SO4) on the solid sample (To evolved
a little solid sample in a test tube add Effervescence and a gas evolved turns
a few drops of conc. H2SO4 and warm lime water milky CO2 evolved
the mixture if necessary.
Blue solid turns white when
concentrated H2SO4 is added without
heating
No gas is evolved
Brick red
Blue
Flame Test
Blue-green or dark green flame
observed
No definite colour seen
Appearance

INFERENCE
Transition elements absent
(Fe3+ Fe2+ Cu2+ )
Cu2+ may be present
Fe2+ may be present
Fe3+ may be present
NH4+ present
Hydrated salt may be present
NH4+ present
Zn2+ may be present
Pb2+ may be present
NO3- present
SO42- present
CO32- present
Cu2+ may be present
Fe3+ may be present
HCO3- or CO32- present
Cl- may be present
NO3- may be present
HCO3- or CO32- present
CuSO45H2O may be present
SO42- may be present
Ca2+ may be present
Pb2+ may be present
Cu2+ may be present
Ca2+ Pb2+ Cu2+ may be absent

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SOLUBILITY OF SUBSTANCES IN WATER:
Ions
Na+ K+ Ca2+
NH4+
2CO3
+
X
+
SO42+
O
+
NO3
+
+
+
OH+
O
No action
Cl+
+
+
Key: + soluble
X insoluble
O sparingly/slightly soluble

Zn2+
X
+
+
X
+

Cu2+
X
+
+
X
+

Fe2+ Fe3+
X
+
+
X
+

Pb2+
X
X
+
X
O

TEST FOR GASES

When doing any experiment do not waste time testing for gases unless you know a gas is being evolved. Gases can
easily be detected by colour, effervescence, and smell. The description below can help you to predict the gas before
even going to specific tests.
a) gas produced has neither colour nor smell could be suspected to be either O2 H2 or CO2
b) Gas produced which is not coloured and has a strong smell could be HCl, SO2 or NH3
c) Gas produced which is coloured could be NO2 if the colour is Brown or Cl2 if the colour is yellowish
green
The table below gives a summary of tests for common gases encountered in qualitative analysis.
Gas
Colour
Smell
Litmus
Other tests
Inference
H2
colourless
None
None
Burns with a pop sound
Metal + acid
O2
Colourless
None
None
Rekindles glowing splint
Metal oxides nitrates
CO2
Colourless
None
Blue to red
Turns lime water milky
Carbonates
NH3
Colourless
Strong Red to blue
White smoke with HCl (g)
Ammonium salt
Cl2
Pale yellow Strong
Blue to red
White fumes with NH3 gas
Chlorides
SO2
Colourless
Strong
Blue to red
Dichromate solution turns green
Sulphates
NO2
Brown
Strong
Blue to red
Nitrates
H2O
colourless
None
None
Cobalt chloride paper changes blue to pink;
Anhydrous copper sulphate changes white
to blue
2) Tests in Solution
Cations
TEST

OBSERVATIONS
Gas with chocking smell and turns damp
litmus paper blue on warming NH3 gas
evolved
White precipitate insoluble in excess
To a sample solution sodium
Blue precipitate insoluble in excess. The
hydroxide is added in small quantities
precipitate turns black on heating
until it is present in excess
Green precipitate insoluble in excess and
turns brown on surfaces
Reddish-brown precipitate insoluble in
excess
White gelatinous precipitate soluble in
excess forming a deep blue solution
To a sample solution aqueous
Green precipitate insoluble in excess
ammonia is added until excess
Reddish-brown precipitate insoluble in
excess is formed

INFERENCE
NH4+ present
Ca2+ present
Cu2+ present
Fe2+ present
Fe3+ present
Cu2+ present
Fe2+ present
Fe3+ present

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3)Confirmation tests
Cations
TEST
1) i) To a sample solution ammonium
oxalate is added
ii) Flame test
iii) A solid sample is warmed with
sodium hydroxide solution
2) a) To a sample solution ammonium
thiocyanate or potassium thiocyanate is
added
b) potassium ferrocyanide is added to
the sample solution
3) a) to a sample solution few drops of
potassium ferrocyanide is added
b) to the solution of the sample NaOH
solution is added
4) a) To a solution of sample ammonia
solution is added until excess
b) To a test solution potassium
ferrocyanide solution is added
5) a) To sample solution potassium
chromate solutions added
b) To a sample solution potassium
iodide solution is added
6) a) To a test solution potassium
ferrocyanide solution is added in excess
b) To a sample solution, NaOH solution
added until in excess

OBSERVATIONS
White ppt insoluble in acetic acid but soluble in
mineral acid
Brick-red flame is observed
Ammonia gas is evolved which turns litmus from
red to blue
a) Deep red solution is observed

INFERENCE
Ca2+ ion confirmed

Fe3+ ion confirmed

b) Blue ppt
a) Deep blue ppt formed
Fe2+ ion confirmed

b) Green ppt formed turning brown

a) pale blue ppt formed. Soluble in excess aqueous
ammonia
b) reddish-brown gelatinous ppt is formed soluble in
aqueous ammonia but insoluble in aqueous mineral
acids
a) Yellow ppt soluble in sodium hydroxide but
insoluble in ammonia solution
b) Yellow ppt is formed. Soluble in excess
potassium iodide solution or on heating but
reappears on cooling.
a) bluish white ppt is formed insoluble in excess
potassium ferrocyanide
b) white gelatinous ppt is formed which is soluble in
excess

Cu2+ confirmed

Pb2+ confirmed

Zn2+ confirmed

Anions
TEST
1. To a sample solution AgNO3 solution
is added followed by dilute HNO3
solution, then excess ammonia solution
2. A sample solution solid is mixed with
manganese dioxide and conc. H2SO4 is
added and warmed
3. To a sample solution dilute HCl is
added followed by BaCl2 solution
4. To a sample solution add freshly
prepared ferrous sulphate solution of
conc. H2SO4 along the side of the test
tube
5. For water insoluble carbonate add
dilute HCl
6. To a solid sample dilute HCl is added
7. To a solution of the sample in water
MgSO4 is added, boiled if no ppt is
formed

OBSERVATIONS
White ppt insoluble in dilute HNO3 but
soluble in ammonia solution
Greenish-yellow gas with pungent smell
(Cl2) is given out which turns moist KI
starch paper blue
White ppt insoluble in dilute HCl is
formed
Brown ring is formed

INFERENCE

Cl- confirmed

SO42- confirmed
NO3- ion confirmed

Effervescence and a colourless gas

evolved turns lime water milky CO2
evolved
Effervescence and a colourless gas
evolved turns lime water milky CO2
evolved
i) White ppt in cold
ii) white ppt after boiling

HCO3- or CO32- confirmed

CO32- confirmed