Experiment No.
01
SYSTEMATIC SEMIMICRO QUALITATIVE ANALYSIS OF SIMPLE INORGANIC SALTS
A. Preliminary Tests:
Experiment
Observation
Inference
I) APPEARANCE
i) Crystalline
i) Salts of Carbonate may be
absent, The salt may contain
Cl; Br; NO3 ; SO42 radicals;
ii) Armorphous (Light fluffy ii) Salts of CO 2 may be
3
powder)
present.
i) Colourless
i) Salts of
II) COLOUR
Mn2 , Fe2 , Cu 2 , Co2 , Ni 2
may be absent.
ii) Pale pink
ii) Salt may contain Mn2
radical
iii) Pale blue
iii) Salt may contain Cu 2
iv) Salt may contain Fe2
radical
iv) Pale green
II) SOLUBILITY TEST:
Water
Cold
Hot
Dilute HCl
Cold
Dilute HNO3
Hot
Cold
Hot
The given salt is soluble in
B. Analysis of acid radiacls:
Experiment
Observation
I) Analysis of I-group Acid
radicals:
a) Salt + Dilute HCl solution a) Brisk Efferverence
colourless gas
b) No Effervesence
The colourless gas is passed
through lime water.
Confirmatory test for CO32
radical:
Salt + Water. Boiled the
vapours are passed through
lime water.
ii) Analysis of II-group acid
radicals
Salt + conc. H 2 SO4
Lime water turns milky
Inference
of a) I-group acid radicals are
present
b) I-group acid radicals are
absent.
Salt may contain CO32 or
HC HCO3 radical
i) Lime water does not turn
milky
ii) Lime water turns milky
i) Fuming gas in cold or hot
condition
ii) No fuming gas either in cold
condition or in hot condition.
iii) No fuming gas in cold
condition
iv) Colourless fuming as in
cold condition which gives
dense white fumes with
glass rod dipped in NH 4OH
1
CO32 radical is confirmed
HCO3 radical is confirmed.
II-group acid radicals are
present.
II-group acid radicals are
absent.
Cl-and Br
radicals
absent.
Cl radical is present
are
solution.
v) Reddish brown fumes in
cold condition and the
solution in the test tube turns
to brown.
vi) Reddish brown fumes
only upon heating.
Liberation of reddish brown
fumes increases upon
heating with copper bits and
the solution in the test tube
becomes greenish blue.
Confirmatory test for Cl
Salt + K 2Cr2O7 crystals + Reddish brown fumes are
liberated
conc. H 2 SO4 heated.
Yellow coloured solution is
Liberated fumes are passed obtained.
through NH 4OH solution
yellow
coloured
Yellow coloured solution + Bright
Acetic acid + Lead acetate precipitate
solution.
Confirmatory test for Cl
and Br radicals.
Silver nitrate test:
Salt solution + dilute HNO3
boiled + Silver nitrate
solution
i) Curdy white precipitate
soluble in NH 4OH
ii) Pale yellow precipitate
soluble in excess NH 4OH
solution.
Confirmatory test for Br
radical.
Globule test:
Salt solution + Chlorine Orange globule is formed.
water + few drops of CCl4
shaken well.
Confirmatory test for NO3
radical:
Brown ring is formed at the
Brown ring test:
Salt solution + Freshly junction of the two liquids
prepared FeSO4 (Mohrs
salt) solution shaken well +
conc. H 2 SO4 along the sides
of the test tube.
Br radical is present
NO3 radical is present.
Cl radical is confirmed
Cl radical is confirmed
Br radical is confirmed
Br radical is confirmed
NO3 radical is confirmed.
c) Analysis of III group acid radical:
(i) Confirmatory test for SO42 :
1) Barium chloride test:
Salt solution + Barium
chloride solution
2) Lead acetate Test: Salt
Solution + Lead acetate
A milky white precipitate III group acid radical present
which is insoluble in excel of SO confirmed.
4
dil. HCl
White precipitate is formed
SO confirmed.
4
(ii) Confirmatory test for Borate BO33
1) Ethyl Borate test: Salt + 2
drops of conc. H 2 SO4 3
drops of ethyl alcohol, heat
& ignite the vapours.
2) Boron trifluoride Test:
Salt + calcium fluoride to
make a paste with 2 drops of
con. H 2 SO4 . The paste is
held in the non-luminous
flame with a glass rod.
The vapours burn with a III group acid radical present
green edged flame
BO3 confirmed.
3
A vivid green colour is
imported to the flame
BO33 confirmed.
Preparation of Original solution: Original solution of the salt is prepared by dissolving 0.3g
of salt in a 10 15 cm3 of suitable solvent. (A few drops of this original solution is used for
basic radical analysis)
I. Analysis of I group basic radical:
Original solution + dil. HCl
No precipitate
I group basic radical absent
II. Analysis of II group basic radical
Original solution + dil HCl No precipitate
H 2 S gas
II group basic radical absent
III. Analysis of III group basic radical:
Original solution + NH 4Cl + Gelatinous white precipitate III group basic radical
formed
present.
Al may be
excess NH 4OH
present
Confirmatory test for Al 3 :
1. Original solution NaOH
solution drop wise.
To the above solution add
solid ammonium chloride
and warm.
2. Original solution +
NH 4OH solution
Gelatinous white precipitate
soluble in excess of NaOH
White precipitate
Gelatinous white precipitate
formed. Insoluble in excess
of NH 4OH
IV. Analysis of IV group basic radical:
Original solution + NH 4Cl + White or flesh coloured
precipitate.
excess NH 4OH H 2 S gas
a) White precipitate
b) Flesh
coloured
precipitate
Al confirmed.
Al confirmed.
IV group basic radical
present
Zn++ may be present
Mn++ may be present
Confirmatory test Zn
1. original solution + NaOH White precipitate soluble in Zn++ Confirmed
drop wise.
excess of NaOH
2. Salt solution + NH 4OH White precipitate soluble in Zn++ confirmed
3
drop wise
excess of NH 4OH
Confirmatory test for Mn++
1. Original solution + NaOH White precipitate insoluble Mn++ confirmed
drop wise
in
excess
of
NaOH
precipitate
turns
brown
slowly when exposed to air
2. Permanganic acid test:
Pink supernatant liquid is Mn++ confirmed
Original solution (dil) + formed
small amount of lead dioxide
+ conc. HNO3 boil, cool and
dilute with water.
V. Analysis of V group basic radical:
Original solution + NH 4Cl White precipitate
excess
V group basic radical
present. It may be Ba or
NH 4OH NH 4 2 CO3
Distinguish test: Original
solution + calcium sulphate
/
Ammonium
sulphate
solution
Confirmatory test for Ba
1. original solution +
potassium chromate solution
2. Flame test: The given salt
is made into a paste with few
drops of conc. HCl. The
paste is held to flame with
the help of previously heated
platinum wire. Observe the
colour imparted to the flame.
(i)
(ii)
Ca
White ppt
No ppt
Ba 2 may be present
Ca 2 may be present
Yellow precipitate
Apple green colour
imparted to the flame
Ba confirmed.
is
Confirmatory test of Ca
1. Original solution + White precipitate
ammonium oxalate solution.
2. Flame test: The given salt
is made into a paste with few Brick red colour is imparted
drops of conc. HCl. The to the flame
paste is held to flame with
the help of previously heated
platinum wire. Observe the
colour imparted to the flame.
IV. Analysis of VI group basic radical:
Confirmatory test for Mg
1. Original solution +
White precipitate
NH 4Cl NH 4OH NH 4 HPO4
White precipitate formed
insoluble in excess of
NaOH
2. Original solution + NaOH
solution
Detection of ammonium radical NH 4 :
Ba confirmed.
Ca is confirmed.
Ca is confirmed.
VI group basic
present.
Mg confirmed.
Mg confirmed
radical
1. Salt + 10% NaOH solution A colourless pungent NH VI group basic radical
3
and heat
present
smelling gas is liberated.
a) It gives dens white fumes
with a glass rod dipped in
con. HCl.
b) The gas turns moist, red
NH 4 may be present.
litmus paper blue
Confirmatory test for NH 4 (Nesslers reagent test):
Original solution + Nesslers A brown coloured
reagent
precipitate is formed
Confirmatory test for Na :
1. Original solution +
potassium pyroantimonate
scratch the inner sides of test
tube with glass rod
2. Flame test: The given salt
is made into a paste with few
drops of conc. HCl. The
paste is held to flame with
the help of previously heated
platinum wire. Observe the
colour imparted to the flame
NH 4 confirmed
White crystalline precipitate
VI group basic
present.
Na confirmed.
Golden yellow colour
imparted to the flame
Na confirmed.
is
Confirmatory test for K :
1. Salt solution + Picric acid Yellow crystalline precipitate VI group basic
solution. Scratch the inner
present.
sides of test tube with glass
K confirmed.
rod.
2. Flame test: The given salt Lilac (violet) colour is
K confirmed.
is made into a paste with few imparted to the flame
drops of conc. HCl. The
paste is held to flame with
the held of previously heated
platinum wire. Observe the
colour imparted to the flame.
radical
radical
5. Report: The given inorganic salt contains
Acid radical
Basic radical
Hence the given salt is _________________
Preparation of Nesslers reagent:
2 or 3 drops of mercuric chloride is taken in a test tube. Potassium iodide solution is added
till scarlet red precipitate formed just dissolve to give a clear solution. Add equal volume of
NaOH solution.
Flame test: The given salt is made into a paste with few drops of conc. HCl. The paste is held
to flame with the help of previously heated platinum wire. Observe the colour imparted to
the flame.
Calcium
Sodium
- Brick red
- Golden yello
Barium
Potassium
-Apple green
- Lilac (violet)