SYSTEMATIC PROCEDURE FOR INORGANIC

SEMIMICRO QUALITATIVE ANALYSIS

S. EXPERIMENT OBSERVATION INFERENCE

No

1 PRELIMINARY TESTS: Green May be Nickel

Color of the substance is noted.

Blue May be copper

Colorless Absence of
copper, Cobalt,
Nickel

2 FLAME TEST:

A little amount of the substance is Bright green May be Copper or

taken in a watch glass and few borate
drops of concentrated
hydrochloric acid are added and
made into paste. The paste is Presence of Barium
taken in a glass rod and Pale green
introduced into the flame. The
color of the flame is noted.
Presence of
Brick red Calcium

3 CALCIUM FLUORIDE
TEST:

The substance is mixed with little

calcium fluoride and conc.
sulphuric and made into paste in a Deep green color Presence of borate
watch glass The paste is
introduced into the flame by
means of glass rod. The color of
the flame is noted.

1
4 TEST FOR CARBONATE: Colorless gas is Presence of
evolved with brisk carbonate
Few drops of dilute hydrochloric
acid are added to substance taken Effervescence.
in a test tube.

5 TEST FOR OXALATE: Colorless gas is

evolved with brisk
Substance + manganese di oxide effervescence. Presence of oxalate
+dil. sulphuric acid and warm.

6 ACTION OF CONC.
SULPHURIC ACID:
Reddish brown Presence of nitrate
A little of the substance is vapors are or bromide
warmed with few drops of conc. evolved
sulphuric acid in a dry test tube.

7 ACTION OF CONC. Reddish brown Presence of

SULPHURIC ACID AND vapor is evolved bromide
MANGANESE DI OXIDE:

Substance + a pinch of
manganese di oxide + conc. Greenish yellow
sulphuric acid and warm the gas is evolved with
pungent smell. Presence of
contents. chloride

8 COPPER TURNINGS TEST: Reddish brown gas Presence of Nitrate.

is evolved and the
Substance + copper turnings+few solution turns pale
drops of conc. sulphuric acid and Green.
warm the contents.

9 ETHYL BORATE TEST

Substance + few drops of ethyl

alcohol + few drops of conc.
Sulphuric acid. Warm the Burns with a green Presence of Borate.
contents and ignite the vapours in edged flame.
the flame.

2
10 AMMONIUM MOLYBDATE
TEST : Substance + few drops of Check your progress
conc. nitric acid, heat and cool
the contents. Then add few drops 1. Why do you see
Canary yellow Presence of effervescence when
of ammonium molybdate ppt. Phosphate. testing for carbonate?
solution.

11 CHROMYL CHLORIDE
TEST:

Little quantity of the substance is

taken in a dry test tube and a
pinch of Potassium dichromate Yellow ppt is got Presence of
and few drops of conc. sulphuric Chloride.
acid are added and heated. The
red orange vapour produced is
passed into water. Yellow
solution is got. To this few drops
of acetic acid and lead acetate are
added.

12 SODIUM HYDROXIDE TEST Colorless gas with Presence of

A little of the substance is heated smell of ammonia
with few drops of sodium is evolved which Ammonium ion
hydroxide solution. gives white dense
fumes with a glass
rod dipped in conc.
hydrochloric acid.

PREPARATION OF SODIUM CARBONATE EXTRACT:

A Small quantity of the substance is taken in a semimicro boiling

tube + thrice the quantity of anhydrous sodium carbonate + 5 ml of
distilled water. Boil the contents for about 10 minutes. It is then cooled
and centrifuged. The centrifugate is known as sodium carbonate extract
and it is used to conduct the following tests.

3
S. No. EXPERIMENT OBSERVATION INFERENCE

1 SILVER NITRATE TEST White curdy ppt Presence of

soluble in NH4OH. Chloride.
A little of the extract is
acidified with dil. nitric acid
till there is no bubbles. It is
then boiled and few drops of Pale yellow ppt partly
silver nitrate soln. is added. soluble in NH4OH.
Presence of
bromide.

2 BARIUM CHLORIDE
TEST

A little of the extract is

acidified with dil. A White ppt insoluble Presence of
hydrochloric acid till in all mineral acid is sulphate.
effervescence stops. It is then got.
boiled and few drops of
barium chloride solution are
added.

3 BROWN RING TEST

The extract is acidified with

dil. sulphuric acid till there is
no effervescence and then
mixed with with few drops of Brown ring is formed Presence of
freshly prepared ferrous at the junction of the nitrate.
sulphate solution. To this liquids.
mixture conc. sulphuric acid
is added carfully along the
sides without shaking the test
tube.

4 CALCIUM CHLORIDE
TEST A white ppt is Presence of
The extract is acidified with obtained oxalate
acetic acid till there is no
effervescence. It is boiled and
few drops of calcium chloride
solution are added.

4
 The ppt is dissolved dil. Pink color is Presence of
sulphuric acid and the decolorized oxalate.
contents are warmed. Now
few drops of dil. potassium
permanganate solution are
added.

Check your progress Check your progress

2. What is the 3. Why the pink color

chemistry behind the of permanganate
brown ring test for decolorizes?
nitrates?

ELIMINATION OF INTERFERING ANIONS AND

PREPARATION OF ORIGINAL SOLUTION

ELIMINATION OF OXALATE: Check your progress

If oxalate is present, a pinch of the substance is roasted in a China dish for 4. What are called
about 10 minutes. The roasted residue is then dissolved in dilute interfering anions?
hydrochloric acid and centrifuged. The residue if any is analyzed for lead.
The centrifugate is used for the analysis of second group and so on.

ELIMINATION OF BORATE:

A Pinch of the substance is taken in a china dish and few drops of

concentrated hydrochloric acid are added. It is then evaporated to
dryness. This process is repeated for 3 times. The residue is dissolved in
dil. hydrochloric acid and centrifuged. The residue if any is analyzed for
lead. The centrifugate is used for the analysis of second group and so on.

ELIMINATION OF PHOSPHATE:

Phosphate has to be eliminated only after the II Group separation. The

centrifugate from the II group is boiled to expel hydrogen sulphide gas
and then few drops of ammonium chloride and zirconium chloride ( or
zirconium nitrate) are added. It is then centrifuged. The residue is
5
 discarded. The process is repeated until no white ppt is obtained by the
addition of zirconyl chloride. The centrifugate is used for the analysis of
III Group and so on.

SYSTEMATIC ANALYSIS OF CATIONS

Check your progress TEST FOR AMMONIUM ION:

5. What is Nessler’s A little quantity of the mixture is taken in a centrifuge tube. One ml of
reagent?
distilled water is added and shaken well. It is then centrifuged .To the
centrifugate few drops of sodium hydroxide and an excess of NESSLER'S
REAGENT is added. A brown precipitate shows the presence of
AMMONIUM ION.

IDENTIFICATION OF GROUPS

S. No. EXPERIMENT OBSERVATION INFERENCE

1 To the original
solution a few drops
of dil. hydrochloric White ppt is got. Presence of Group I
acid is added and
centrifuged.

2 The centrifugate is Black or brown ppt. Presence of Group II

heated,

Hydrogen sulphide
gas is passed and
centrifuged.

3 The centrifugate
from the above is
boiled. Few drops of
ammonium chloride White ppt Presence of Group III
and excess of
ammonium
hydroxide are added
and centrifuged.

6
4 The above White ppt or
centrifugate is flesh colored ppt or Presence of Group IV
Boiled, cooled and Black ppt
hydrogen Sulphide
gas is passed and
centrifuged.
5 The centrifugate is
boiled and cooled.
Few drops of
ammonium chloride, White ppt Presence of Group V
ammonium
hydroxide and
Ammonium
carbonate are added
and centrifuged.

6 The centrifugate from

group V is concentrated
by boiling. Few drops
of conc. nitric acid are
added and evaporated
till no more fumes are
evolved. The residue is
extracted with water.
To the solution few
drops of ammonium
hydroxide and an White crystalline ppt. Presence of Mg
excess of Sodium
phosphate solutions are
added, shaken and the
sides of the test tube are
rubbed with a glass rod.

Check your progress

6. What is common and

different with the reagents
used for II and IV groups?

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 ANALYSIS OF GROUP I METALS

The ppt obtained in group 1 is boiled with 5 ml of water and

centrifuged while hot. The centrifugate is divided into 2 portions.

1) To the first portion, few drops of acetic acid and few drops of
potassium chromate are added. Yellow ppt is got-PRESENCE OF
LEAD.

2) To the second portion, few drops of potassium iodide solution are

added. Yellow ppt is got. This ppt is heated with 10 ml of water and
cooled.

Golden yellow spangles appear - PRESENCE OF LEAD.

ANALYSIS OF GROUP II METALS [Pb, Bi, Cu]

The GROUP II residue is washed with water and boiled with 2 drops of
dil. nitric acid and 2 drops of dil. sulphuric acid and centrifuged.

RESIDUE CENTRIFUGATE

This is boiled with a few To the centrifuate, ammonium hydroxide is

drops of ammonium acetate added in excess and centrifuged.
solution and divided into 2
parts. RESIDUE CENTRIFUGATE

Residue is dissolved in To one portion of

To one part, added 2 drops
of potassium chromate
solution.
Yellow ppt-presence of
lead.
To another portion,
potassium
Minimum amount of the centrifugate, few
dilute hydrochloric acid drops of acetic acid
and divided into 2 and few drops of
parts. Potassium ferro
cyanide are added.
To the first part, little
water is added. White Brown color ppt-
turbidity –Presence of presence of copper
BISMUTH.

Iodide solution is added.

8
 The yellow ppt obtained is
boiled with 10 ml of water
– Golden yellow spangles
– presence of lead.
To the second part,
little amount of
thiourea and few drops
of dil. nitric acid are
added. Yellow color –
presence of bismuth.

ANALYSIS OF GROUP III METALS [Al]

The third group ppt is boiled with about 5ml of water and little sodium Check your progress
peroxide till the liberation of oxygen stops. It is diluted and centrifuged.
7. Can you draw the
A portion of the centrifugate is acidified with dil. hydrochloric acid.
structure of Ni-DMG
Ammonium hydroxide solution is added in excess and allowed to stand for complex?
few minutes. White gelatinous precipitate – presence of aluminium.

ANALYSIS OF GROUP IV METALS [Ni, Co, Zn, Mn]

The IV Group ppt is washed with water and shaken with 1 ml of dil. HCl
and 4ml of water. The mixture is then centrifuged.

RESIDUE CENTRIFUGATE

This is dissolved in conc. Hydrogen sulphide is boiled off and sodium

hydrochloric acid and a crystal of hydroxide solution is added in excess and
potassium chlorate is added and centrifuged.
evaporated to dryness in a china
dish. The mass is dissolved in little
water and divided into 3 parts. RESIDUE CENTRIFUGATE

9
 White ppt This is divided into 2 parts.
turning brown is
To the first part, 2 drops of got. This is
ammonium chloride, 4 drops of shaken with a
ammonium hydroxide and 4 drops of To one portion Hydrogen
pinch of sodium sulphide gas is passed.
Potassium ferricyanide solutions are bismuthate and 2
added. Reddish brown color or ppt to 4 drops of White ppt - presence of
– presence of cobalt. dil.nitric acid. Zinc.

Pink Color-
To the second part, Little solid presence of
The ppt is dissolved in conc.
ammonium thio cyanate is added nitric acid and few drops
Manganese.
followed by a few drops of amyl cobalt nitrate solutions are
alcohol and ether .It is shaken well. added. A filter paper is
dipped in this solution and
Blue layer-presence of Cobalt
burnt.

Green ash is got-presence

To the third part, 2 drops of of Zinc
ammoniumchloride 4 drops of
ammonium hydroxide and 4 drops
of dimethyl glyoxime Solutions are The second part is acidified
added. Rosy red ppt-presence of with acetic acid and 2 drops
Nickel. of potassium ferrocyanide
solution is added.

White ppt is got-presence

of Zinc.

10
 ANALYSIS OF GROUP V METALS [ Ba, Ca, Sr]

The V GROUP ppt is dissolved in warm acetic acid. Potassium

chromate solution is added in slight excess, boiled and centrifuged.

RESIDUE CENTRIFUGATE

Yellow residue is got. This is made To a portion of centrifugate few

in to a paste with conc. hydrochloric
acid and flame test is conducted.
Pale green color-presence of
Barium
drops of ammonium hydroxide and 4
drops of ammonium oxalate solution
are added.White ppt-presence of
Calcium.

TEST FOR MAGNESIUM

To the original solution, add solutions of ammonium chloride, ammonium

hydroxide and di sodium hydrogen phosphate. White pp – Presence of
Magnesium.

Check your progress

8. Why do you see a

white ppt when you
add sodium hydrogen
phosphate to a
solution of Mg2+ ions?

11