SYSTEMATIC SEMI-MICRO QUALITATIVE ANALYSIS OF AN INORGANIC SALT.

1. PRELIMINAY OBSERVATIONS:
a) State: Amorphous ; carbonates or borates
Crystalline ; chlorides, sulphates, nitrates.
b) Color: Blue; copper salts
dark brown; ferric salts
light green; ferrous salts
pale pink; manganous salts.
c) Odor: ammoniacal smell; ammonium salt.
d) Solubility test: take 0.02-0.03 g of the given salt in the test tube. Add 1-2 ml of one of the
following solvents in the order given below, to get a clear solution. Try the solubility in cold
solvent, if partially soluble, warm to dissolve completely.
solvent

Water
Cold
Hot

Dil.HCl
Cold
Hot

Conc.HCl
Cold
Hot

Dil.HNO3
Cold
Hot

Conc. HNO3
Cold
Hot

solubility

2. ANALYSIS OF ACID RADICALS [ANIONS]:

GROUP-I
EXPERIMENT
Salt + dil.HCl

OBSERVATION
a) Brisk effervescence takes
place with the evolution of
colourless gas.
b) colourless gas is not
liberated

INFERENCE
a) May be CO32- or S2- or SO32or NO2-.
b) Group-I acid radicals are
absent.

CONFIRMATORY TEST FOR GROUP-I RADICALS.

EXPERIMENT
i) Salt + dil.HCl. Pass the gas
through lime water.

OBSERVATION
Lime water turns milky.

INFERENCE
CO3 or SO32- is present.
2-

ii) salt + a few drops of

acidified KMnO4.

iii) salt + water + BaCl2

solution.
iv) salt + water + acetic acid+
lead acetate solution.
v) salt + water + acetic acid +
FeSO4.

a) pink color of KMnO4 is

retained.
b) pink color of KMnO4
disappears.
White ppt is formed which
dissolves in dil.HCl.
Black ppt

a) CO32- is confirmed.

Dark brown or black colour is

obtained.

NO2- Is confirmed.

OBSERVATION
a) Colorless gas is liberated.
b) Brown fumes are evolved
and the solution turns brown.
c) Violet gas or vapours are
evolved with black deposits in
the inner side of test tube.
d) Colorless fumes with slight
brown gas but the solution is
not brown.
e) Colorless, odorless gas.
f) Colorless vapours with
vinegar smell.

INFERENCE
a) May be chloride.
b) May be bromide.

b) SO32- or S2- is present.

SO32- Is confirmed.
S2- Is confirmed.

GROUP-II
EXPERIMENT
Salt + Conc.H2SO4. Warm if
necessary.

c) May be iodide.
d) May be nitrate.

e) May be oxalate.
f) May be acetate.

CONFIRMATORY TEST FOR GROUP-II RADICALS.

EXPERIMENT
C.T for Cl- :
i) Chromyl Chloride test:
Salt + K2Cr2O7 crystals +
conc.H2SO4. heat & pass the
vapours through a t.t
containing little water.
Above yellow solution +
NaOH + acetic acid + lead
acetate.
ii) Silver nitrate test:
Salt + dil.HNO3 + AgNO3

OBSERVATION
Red vapours are evolved.

INFERENCE
Cl- is present.

Water turns yellow.

Yellow ppt is obtained.

Cl- is confirmed.

Curdy white ppt soluble in

Cl- is confirmed.

solution.
EXPERIMENT
C.T for Br-:
i) Silver nitrate test:
Salt + dil.HNO3 + AgNO3
solution.
ii) Globule Test:
Aq. Soln of the salt + chlorine
water + 2 drops of CCl4. Mix
well.
EXPERIMENT
C.T for I-:
i) Silver nitrate test:
Salt + dil.HNO3 + AgNO3
solution.
ii) Globule Test:
Aq. Soln of the salt + chlorine
water + 2 drops of CCl4. Mix
well.
EXPERIMENT
C.T for NO3-:
i) Salt + copper + conc.H2SO4
+ heat.
ii) Brown Ring Test:
Aq. Soln of the salt + Conc.
H2SO4 + cool & add freshly
prepared FeSO4.
EXPERIMENT
C.T for CH3COOi) oxalic acid test:
Salt + oxalic acid + 2-3 drops
of water, rub.
ii) ester test:
Salt + conc.H2SO4 + ethyl
alcohol. Heat.

NH4OH is obtained.
OBSERVATION

INFERENCE

Pale yellow ppt slightly

soluble in NH4OH is obtained.

Br- is confirmed.

A brown Globule is formed.

Br- is confirmed.

OBSERVATION

INFERENCE

Yellow ppt insoluble in

NH4OH is obtained.

I- is confirmed.

A violet Globule is formed.

I- is confirmed.

OBSERVATION

INFERENCE

More brown fumes are

evolved and the solution turns
blue..

NO3- is confirmed.

A brown ring is formed at the

junction of the two liquids.

NO3- is confirmed.

OBSERVATION
Vinegar smell.

INFERENCE
CH3COO- is confirmed.

Fruity smell of an ester.

CH3COO- is confirmed.

EXPERIMENT
C.T. for C2O42- :
i) Salt soln + acetic acid +
CaCl2 solution.
ii) Salt + dil.H2SO4, warm and
add 2-3 drops of KMnO4
solution.

OBSERVATION

INFERENCE

White ppt is formed.

C2O42- is confirmed.

Pink color is discharged.

C2O42- is confirmed.

GROUP-III
Test for sulphate:
EXPERIMENT
i) Barium Chloride Test:
Soln.of the salt + barium
chloride soln + dil.HCl.
ii) Match Stick Test:
mix the salt with Na2CO3.
Make its paste. Fuse a little
paste on the end of match
stick. Dip the fused mass in
sod.nitroprusside solution.

OBSERVATION
A white ppt insoluble in
dil.HCl is obtained.

INFERENCE
SO42- is confirmed.

Purple steaks.

SO42- is confirmed.

OBSERVATION
Yellow ppt is formed in cold
or on slight warming.

INFERENCE
PO43- is confirmed.

White ppt is formed.

PO43- is confirmed.

Test for phosphate:

EXPERIMENT
i) Ammonium Molybdate
Test: Salt + con.HNO3, boil
well, till no brown gas is
evolved, cool & add excess of
Ammonium Molybdate
solution.
ii) Magnesia mixture test:
salt + water + magnesia
mixture.

3. ANALYSIS OF BASIC RADICALS [CATIONS]:

Preparation of original solution(O.S):

A small amount of the salt is dissolved in a suitable solvent to get a clear solution which is called
Original Solution.
GROUP-ZERO:
Test for NH4+:
EXPERIMENT
A] Salt + NaOH solution.
Boil.
a) expose a glass rod dipped in
HCl to the gas.
b) Expose a moist red litmus
paper to the gas.
B] NESSLERS REAGENT
TEST: O.S + Nesslers reagent
+ NaOH solution.

OBSERVATION
Pungent smelling gas is
evolved.
Dense white fumes are
observed.
red litmus paper turns blue.

INFERENCE
NH4+ is present.

A brown ppt is obtained.

NH4+ is confirmed.

OBSERVATION
a) no white ppt
b) a white ppt is formed.

INFERENCE
a) 1st group cations are absent.
b) 1st group cations are
present. May be Pb2+.

A yellow ppt is formed.

Lead is confirmed.

Yellow ppt is formed.

Ppt dissolves and reappears as
golden yellow spangles.

Lead is confirmed.

OBSERVATION
a) no ppt
b) a black or yellow ppt is
obtained.

INFERENCE
a) 2nd group cations are absent.
b) 2nd group cations are
present. [If black, May be Pb2+
or Cu2+. If yellow, may be
As3+].

NH4+ is present.
NH4+ is present.

GROUP-I
EXPERIMENT
O.S + dil.HCl.

C.T for LEAD:

i) O.S + potassium chromate
solution.
ii) O.S + KI solution.
Yellow ppt + water. Boil
& cool.
GROUP-II
EXPERIMENT
O.S + dil.HCl, warm. Pass
H2S gas through the solution.

BLACK PPT:
Heat the black ppt with

min.quantity of 50% HNO3 till

the ppt dissolves. Divide the
solution into two parts.
To one part of the solution
a) white ppt is obtained.
add dil.H2SO4 and alcohol.
b) no white ppt.
To the second part add
NH4OH in excess.
a) blue solution.
b) no blue solution.
C.T for LEAD:
i) O.S + potassium chromate
A yellow ppt is formed.
solution.
ii) O.S + KI solution.
Yellow ppt is formed.
Yellow ppt + water. Boil
Ppt dissolves and reappears as
& cool.
golden yellow spangles.
C.T for Cu2+:
i) to one part of the blue
solution add acetic acid and
potassium ferrocyanide
solution.
ii) to another part add acetic
acid and pot.iodide solution.

a) Pb2+ is present.
b) Pb2+ is absent. May be Cu2+.
a) Cu2+ is present.
b) Cu2+ is absent.
Lead is confirmed.
Lead is confirmed.

A chocolate brown ppt is

formed.

Cu2+ is confirmed.

A white ppt is formed in

brown colored solution.

Cu2+ is confirmed.

A yellow ppt is obtained.

As3+ is confirmed.

A white ppt is obtained.

As3+ is confirmed.

OBSERVATION
a) no ppt.

INFERENCE
a) 3rd group cations are absent.

YELLOW PPT:
Dissolve the yellow ppt in
conc.HNO3 and divide it into
two parts.
C.T for As3+:
i) to the first part of the
solution add ammonium
molybdate solution and heat.
ii) to the second part of the
solution add NH4OH solution
and magnesia mixture.
GROUP-III
EXPERIMENT
O.S + conc. HNO3. Boil for

some time. Add NH4Cl and

boil again. Cool the solution
under tap water and add
excess of amm.hydroxide.
C.T for Al3+:
i) LAKE TEST:
dissolve a part of the ppt in
dil.HCl. add 2 drops of blue
litmus solution, then add
amm.Hydroxide dropwise till
the blue colour develops.
ii) dissolve the remaining ppt
in NaOH and add
amm.chloride solution to it.
C.T for Fe3+:
Dissolve the brown ppt in
dilute HCl, and divide the
solution into two parts.
i) POTASSIUM
FERROCYANIDE TEST:
to one part of the solution
add potassium ferrocyanide
solution.
ii) POTASSIUM
SULPHOCYANIDE TEST:
to the second part add a
little potassium sulphocyanide
solution.

b) if white ppt.
if brown ppt.

b) 3rd group cations are

present. May be Al3+.
May be Fe3+.

blue ppt floating in the

colorless solution.

Al3+ is confirmed.

Gelatinous white ppt

reappears.

Al3+ is confirmed.

Prussian blue colouration.

Fe3+ is confirmed.

Blood red coloration.

Fe3+ is confirmed.

OBSERVATION
a) no ppt.
b) ppt is obtained.
If black ppt.
If buff (flesh) colored ppt.
If dull white ppt.

INFERENCE
a) 4 group cations are absent.
b) 4th group cations are present
may be Co2+ or Ni2+.
May be Mn2+.
May be Zn2+.

GROUP-IV
EXPERIMENT
O.S + conc. HNO3. Boil for
some time. Add NH4Cl and
boil again. Cool the solution
under tap water and add
excess of amm.hydroxide
solution and pass H2S gas.

th

BLACK PPT:
Observe the color of the
original solution. If the salt is
purple or deep violet in color
perform C.T for Co2+ and if it
is greenish, perform C.T for
Ni2+ with the original salt.
C.T for Co2+:
i) POTASSIUM NITRITE
TEST:
O.S + amm hydroxide + acetic
acid + a crystal of potassium
nitrite, warm the solution.
ii) AMM. THIOCYANATE
ETHER TEST: O.S + ether +
a crystal of amm. Thiocyanate,
shake the test tube. Allow to
settle.
C.T. for Ni2+:
i) Dimethyl glyoxime test:
O.S + amm. Hydroxide + few
drops of Dimethyl glyoxime.
ii) sodium hydroxide- Br2 test:
O.S + NaOH in excess + Br2
water. Boil.
BUFF colored PPT:
C.T for Mn2+:
i) sodium hydroxide- Br2 test:
O.S + NaOH, shake the
solution.
To the white ppt add Br2
water.
ii) lead peroxide test:
to the black ppt obtained in
the above test add conc.HNO3
and lead peroxide. Boil, cool
and allow to settle.

A yellow ppt is formed.

Co2+ is confirmed.

Blue color in ethereal layer.

Co2+ is confirmed.

Bright rose red ppt is

obtained.

Ni2+ is confirmed.

Ni2+ is confirmed.
A black ppt is formed.

Mn2+ is confirmed.
A white ppt is formed.
It turns black or brown.

Mn2+ is confirmed.
Pink-colored solution is
formed.

DULL WHITE PPT:

C.T for Zn2+:
i) NaOH test:
O.S + NaOH solution
dropwise.
To the white ppt add excess
of NaOH solution.
ii) Pot.ferrocyanide test:
O.S + Pot.ferrocyanide
solution.

A white ppt is formed.

Zn2+ is confirmed.
White ppt dissolves.
Zn2+ is confirmed.
White or bluish white ppt is
formed.

GROUP-V
EXPERIMENT
O.S + NH4Cl, boil, cool and
add NH4OH in excess, then
add (NH4)2CO3 solution.

OBSERVATION
a) no ppt.
b) a white ppt is formed.

INFERENCE
a) 5th group cations are absent.
b) 5th group cations are
present. May be Ba2+ ,Sr2+ or
Ca2+.

A yellow ppt is formed.

Ba2+ is confirmed.

Apple green or grassy green

flame is observed.

Ba2+ is confirmed.

Dissolve the ppt in hot

dil.acetic acid and divide it
into 3 parts.
C.T for Ba2+:
i) potassium chromate test:
one part of the solution + few
drops of potassium chromate
solution.
ii) Flame test:
Make a paste of the original
salt in conc.HCl on a watch
glass. Take a clean Pt wire and
heat it in the non-luminous
flame of the burner till no
color is imparted to the flame.
Take the salt paste on the loop
of the Pt wire and introduce it
into the flame. Note the color
imparted to the flame.

C.T for Sr2+:

i) amm. Sulphate test:
second part of the solution +
amm. Sulphate solution.
Warm.
ii) Flame test:
Make a paste of the original
salt in conc.HCl on a watch
glass. Take a clean Pt wire and
heat it in the non-luminous
flame of the burner till no
color is imparted to the flame.
Take the salt paste on the loop
of the Pt wire and introduce it
into the flame. Note the color
imparted to the flame.
C.T for Ca2+:
i) amm. Oxalate test:
third part of the solution +
amm.oxalate solution + few
dops of amm hydroxide.
Scratch the sides of the test
tube.
ii) Flame test:
Make a paste of the original
salt in conc.HCl on a watch
glass. Take a clean Pt wire and
heat it in the non-luminous
flame of the burner till no
color is imparted to the flame.
Take the salt paste on the loop
of the Pt wire and introduce it
into the flame. Note the color
imparted to the flame.

A white ppt is formed.

Sr2+ is confirmed.

Crimson red flame is

observed.

Sr2+ is confirmed.

A white ppt is formed.

Ca2+ is confirmed.

Brick red flame is seen.

Ca2+ is confirmed.

GROUP-VI
EXPERIMENT
C.T for Mg2+:

OBSERVATION

INFERENCE

i) amm.phosphate test:
O.S + solid NH4Cl + NH4OH
solution in slight excess. Add
amm phosphate solution and
scratch the sides of the test
tube with a glass rod.

A white ppt is formed.

Mg2+ is confirmed.

RESULT:
The given salt contains ___________ as acid radical(anion) and _____________ as basic
radical (cation). Hence the given salt is _____________.