Systematic Procedure for Inorganic Qualitative Analysis

Systematic Analysis of Anion

S.No Experiment Observation Inference
1 Preliminary Reactions Colourless Absence of Fe2+, Fe3+, Ni2+,
Co2+.
Appearance Green May be Fe2+, Ni2+, Cu2+
Blue Cu2+
Brown May be Fe2+
Pink May be Co2+, Mn2+
A colourless gas with a May be NH4+ salt
characteristic pungent
Action of heat odour turning moist red
Take a small amount of litmus paper blue.
the given salt taken in a Reddish brown vapours May be
2
dry test tube, heat it turning acidified ferrous
gently; then strongly. sulphate paper brown, are
obtained.
Substance is white when May be (Zn)2+
cold and yellow when hot.
3 Flame Test (i) Bluish green flame May be Cu2+
To a small amount of the (ii) Apple green May be Ba2+
given salt taken in a (iii) Brick red May be Ca2+
watch glass, add a drop (iv) Crimson red May be Sr2+
of Con. HCl and make it
into a paste. Introduce
the paste with the help
of a glass rod to the base
of the non-luminous
bunsen burner.
Identification of Anions from Volatile Products:
Brisk effervescence of Anion is CO32-
colourless, odourless gas
turning lime water, milky is
obtained.
Colourless gas with a smell Anion is sulphide.
of rotten eggs, turning lead
acetate paper black is
obtained.
Colourless gas with smell of Anion is SO32-
burning sulphur turning
Action of dilute H2SO4:
acidified dichromatic green
To a small portion of the
is obtained.
given salt taken in a test
4 Reddish brown gas with Anion is
tube add 1 or 2ccs of
fishy odour turning
H2SO4 and gently warm
acidified ferrous sulphate
it.
brown is obtained.
Colourless gas with smell of Anion may be acetate.
vinegar is obtained.
No characteristic Absence of CO32-, , S2-,
observation. SO3 , CH3COO
2- -
 Reddish brown vapours Anion may be bromide.
turning moist fluorescent
paper red.
Colourless gas with Anion may be chloride.
pungent smell giving dense
Action of Con.H2SO4 white fumes with a glass
To a small amount of rod dipped in NH4OH
given salt taken in a test solution.
5
tube, add 2-3 ccs of Violet coloured vapours Anion may be Iodide.
Con.H2SO4 and gently turning starch paper blue
heat it. or violet.
Reddish brown vapours Anion may be nitrate.
turning acidified ferrous
sulphate paper brown.
No characteristic Absence of , , &
observation.
6 Action of Con.H2SO4 with Copius evolution of reddish Anion is nitrate.
Cu turnings: brown gas turning acidified
Mix a small amount of ferrous sulphate paper
the given salt taken in a brown is observed.
test tube with a few Cu
bits, add 2 – 3 ccs of No reddish brown vapours. Absence of
H2SO4 and heat it.
A greenish yellow gas Anion may be chloride.
Action of Con.H2SO4 with turning starch iodide paper
MnO2 violet (or) blue is obtained.
To a small amount of the Reddish brown vapours Anion may be bromide.
given salt taken in a test turning moist fluorescent
7 tube, add an equal paper red is obtained.
amount of MnO2 and Violet vapours turning Anion may be iodide
add a few ccs of starch paper blue (or) violet
Con.H2SO4 and gently is obtained.
heat. No characteristic coloured Absence of , ,
vapours are obtained.
8 Action of NaOH A colourless gas with a Cation is ammonium.
To a pinch of the given pungent smell giving dense
salt taken in a test tube, white fumes with glass rod
add few ccs of 10% dipped in HCl is obtained.
NaOH solution and
gently warm it. No characteristic gas is Ammonium is absent.
Ammonium liberated.
Sodium Carbonate Extract
Identification of Anions in solution
Preparation of Extract:
Take about or of the given salt in a 50cc beaker. Mix it well with about
thrice its amount of solid sodium carbonate. Add about 15 – 20ml of distilled
water. Mix well with neat glass rod. Boil contents of the beaker over Bunsen
flame. Cool and filter through filter assembly. Collect the clean filtrate in
another beaker. The Filtrate is called soda extract.
S.No Experiment Observation Inference
9 Silver Nitrate Test: Curdy white precipitate Anion is Cl–
To a portion of extract soluble in NH4OH.
add dilute HNO3 until
–
effervescence ceases. Pale yellow precipitate Anion is Br
Add few drops in excess, sparingly soluble in NH4OH.
2 – 3nos of AgNO3
solution. Yellow precipitate insoluble Anion is
in NH4OH.

No precipitate is obtained. Absence of Br–, Cl–, I–

10 Barium Chloride Test: A white precipitate Anion is
To about one or two ccs insoluble in HCl.
of the extract, (after
neutralizing with acetic A white precipitate soluble Anion is
acid and boiling of CO2) in HCl.
add BaCl2 solution.
To a portion of the above No precipitate is obtained. Absence of
ppt add dil. HCl.

11 Lead Acetate Test:

To about one or two ccs White ppt, soluble in excess confirmed.
of the extract (after of ammonium acetate
acidifying with acetic solution.
acid, boiling off CO2 and
cooling) add lead acetate
solution.
12 Ferrous Sulphate Test:
(Brown Ring Test)
To about 1 or 2cc of A brown ring is obtained at Anion is
extract add dilute the junction of the liquid.
H2SO4 in drops until the
effervescence ceases.
And few drops in excess
add 2- 3 drops of freshly No brown ring is observed. Anion is absent.
prepared FeSO4 solution.
Keeping the test tube in
a slanting position, add
Con. H2SO4 without
disturbing the solution.
13 Ferric Chloride Test:
Take about 1 or 2ccs of Deep red colouration confirmed.
the extract in a test tube produced
and add neutral FeCl3
solution. Filter, if
required, and divide the
solution or the filtrate in
two parts:

(i) To one part add Red colouration disappears confirmed.

dil.HCl

(ii) To the second part Reddish brown ppt. confirmed.

add water and boil
14 Calcium Chloride Test:
To a portion of the A white precipitate of Confirms Oxalate.
sodium carbonate calcium oxalate is obtained
extract, taken in a test
tube add dil. Acetic acid
and boil off CO2. Then
add a few drops of
calcium chloride
solution.

Add dil. HNO3 to the The precipitate dissolves.

white ppt and warm.
15 Ethyl Acetate Test:
To a pinch of given salt A pleasant fruity odour is The presence of anion acetate is
taken in a test tube, add obtained. confirmed.
a few drops of ethanol
followed by 1 or 2ccs of
H2SO4. Gently heat and
cool it. Pour into
Na2CO3.
 Systematic Analysis of Cations
Preparation of Original solution:
Check solubility of the given salt in:
- Cold water (or) hot water (or) Dil HCl (or) Conc. HCl. Label this solution as
original solution.

Procedure for Separation of Basic Radicals into Groups

To the original solution, add Dil. HCl.

White ppt.
Group I
present (Pb 2+

and
If no ppt. pass H2S through the given solution. If a coloured ppt. is formed,
group 2 cations are present (Cu2+), Pb2+.
If no ppt is obtained from the above, boil off H2s gas and add a
few drops of conc. HNO3 to the remaining solution. Cool, add
2-3g of solid NH4Cl. Boil again and add NH4OH solution till it
becomes alkaline.
If a ppt is formed, Group III cations are present. Reddish
brown ppt. Fe3+ Gelatinous white ppt. Al3+

If no ppt., pass H2S to the given solution.

If a ppt is formed Group IV cations are

present. Black ppt. (Co2+, Ni2+)
Flesh coloured ppt. Mn2+ white ppt. Zn2+.
If no ppt is formed, boil off
H 2S gas add (NH4)2CO3
solution.
If a white ppt is formed Group
V cations are present (Ba2+,
Sr2+, Ca2+)
If no ppt.
Group VI
cation is
present (Mg2+

If none of the cations are present, check for Group 0 ( )

Cation Analysis

Group O (NH4+):

To a pinch of given salt add Yellowish brown precipitate Cation is ammonium.

some water and warm. is obtained.
Then allow it to cool. Add
Nessler’s reagent and No precipitate is obtained. Cation is not ammonium.
excess of NaOH solution.
Group I (lead):
Group I precipitate is dissolved by heating the precipitate with dil.HNO3 or distilled
water. Divide the solution into 3 portions and carry out the following reactions.
Experiment Observation Inference
To one portion of the above A white precipitate of Pb2+ is present.
solution add dilute H2SO4. PbSO4 is obtained.

To another portion, add A yellow precipitate of Presence of is

potassium chromate is obtained. confirmed.
solution.

Golden Spangles Test: A yellow precipitate is The presence of is

To the 3rd portion, add KI obtained. confirmed.
solution

To above yellow precipitate, Precipitate dissolves and

add some H2O, boil and reappears in the form of
then cool. golden spangles.

Group II ( :
The group 2 precipitate is dissolved by heating with dilute HCl. Precipitate dissolves.

Experiment Observation Inference

Test for :
To one portion of the above A pale blue precipitate The presence of Cu2+ is
solution add drops of which dissolves in excess confirmed.
NH4OH, until it is in NH4OH to give any inky
excess. blue solution is obtained.

To another portion, add

dilute acetic acid and A chocolate brown ppt. Confirms copper.
potassium ferrocyanide
[K4(Fe(CN6))]

Group III:
Group III precipitate is heated with Con. HCl and water, cooled and filtered.
Reddish brown precipitate indicates Fe2+ (or) Fe3+
Gelatinous white indicates Al3+

Experiment Observation Inference

1. To 1 cm3 OS, add a Formation of a deep Fe2+ confirmed.
few drops of dilute blue colour or ppt.
HCl and then add
 0.5 cm3 of potassium
ferricyanide solution.
2. White gelatinous Formation of a blue Al3+ confirmed.
precipitate dissolves floating ppt. in
in minimum quantity colourless solution.
of dil. HCl. To this, (This is known as Lake
add a few drops of test)
blue litmus solution.

Add NH4OH solution A blue ppt., suspended

in excess. in a colourless medium
(called a lake)

2B To one part of the White Precipitate soluble Al3+ confirmed

above solution add in excess of NaOH
NaOH solution solution

3. Reddish brown ppt. A yellow solution is may be present.

(Shows the presence produced.
of Fe3+) Treat it with
minimum quantity of
dil. HCl solution to
dissolve the ppt. and
then heat. Divide the
solution into two
parts.
(i) To one part, add few A deep blue colour or confirmed.
drops of potassium ppt. is obtained.
ferrocyanide solution.

(ii) To another portion A deep red colour is confirmed.

add few drops of obtained.
potassium
sulphocyanide
solution.

Group IV :

Group IV precipitate is warmed with dilute HCl centrifugate

Black precipitate Ni2+
Ni is not soluble in dilute HCl. To residue A Red rosy precipitate confirms the
add Con.HCl, boil, cool. Divide the presence of Ni2+
solution into two parts and boil of H2S. To
one part add dimethyl glyoxime reagent.
Con.NH4OH, till the solution becomes
alikaline.
Sodium Hydroxide and Br2 – water test. A black precipitate confirms the presence
To the second part of the above solution, of Ni2+.
add NaOH and Br2 water and then boil
Confirmation of Zn2+:
Dissolve a part of white ppt in dil. HCl.
Boil off H2S and divide the solution in two
parts. Bluish White ppt confirms Zinc.
(i) To one part of solution add Pot.
ferrocyanide solution
White ppt soluble in excess of NaOH is
(ii) To second part of solution add NaOH.
obtained.
Flesh (buff) colour precipitate indicates A white precipitate is formed. Add Br
Mn2+. water to the white ppt it turns black or
Dissolve the precipitate in Dil. HCl and brown. Mn2+ confirmed.
boil off H2S then add NaOH solution.
Lead peroxide test A pink colouration is produced. Mn2+ is
To the second part of the flesh coloured confirmed.
ppt, add a little of PbO2 powder and
conc. HNO3. Boil, cool and allow to
stand.

Group V :
Take a small portion of Group V precipitate, carry out flame test. Take group V
precipitate, add dilute CH3COOH, warm. Boil of CO2 and divide the solution into
three parts.

Barium, Ba2+ Stronium Sr2+ Calcium Ca2+

1. Potassium chromate
test.
To one part of the above
solution, add a few drops of
K2CrO4 solution – Yellow
ppt. Ba2+ confirmed.
1. Ammonium sulphate 1. Ammonium oxalate test.
test. To the third portion of the
To the second part of the above solution, add
above solution add a few ammonium oxalate
drops of ammonium solution and then NH4OH
sulphate solution – white solution to make it alkaline
ppt. Sr2+ confirmed. and scratch the sides of
the test tube – white ppt.
Ca2+ confirmed.

2. Dil. H2SO4 Test Flame test Flame test

To another portion of the
above solution, add a few
drops of dil. H2SO4 – white
ppt. insoluble in HCl.
Ba2+ confirmed.
Test for Mg2+:

1. Ammonium phosphate test. White crystalline ppt.

To the original salt solution, add solid
NH4Cl, warm to dissolve, cool and add
NH4OH solution in slight excess. Then
add ammonium phosphate solution,
shake well and allow to stand
2. To the original sat solution, add White crystalline ppt confirms Mg2+
disodium hydrogen phosphate.

Additional Test:
Ash test for Al3+, Zn2+, Mg2+

To a pinch of given salt Blue tinted ash is obtained. The presence of Al3+ is
taken in a test tube, add a confirmed.
few drops of Con.H2SO4, Green tinted ash is
Co(No3)2. Mix it well. Dip obtained. The presence of Zn2+ is
one filter paper bit in a confirmed.
Bunsen flame. After it Pink tinted ash is obtained.
burns remove it from The presence of Mg2+ is
flame. After cooking confirmed.
observe the odour of the
ash formed.
 READY REFERENCE CHART FOR QUALITATIVE ANALYSIS OF BASIC RAIDCALS
Make the solution of the given salt in distilled water, in dil. HCl or conc. HCl, cold or hot. Label it original solutions (O.S.). To the O.S., add dil. HCl
White ppt.
2+ If Group I is absent, pass H2S gas through O.S. for sufficient time after acidification with dil. HCl filter.
(Pb ) PPt. - Group II
2+ 2+ If Group II is absent, add solid NH4Cl, 0.5 ml conc. HNO3 to the O.S. Boil and cool. Add NH4OH till it smells of ammonia. If a ppt. is formed, group III is present.
Confirmation
2+ Black ppt. - (Pb , Cu ) Reddish brown ppt. -
of Pb 3+ 3+ If group III is absent, through a part of the solution obtained in group III pass H 2S gas. If a ppt. is obtained group IV is present.
Yellow ppt. - (As ) (Fe ) 2+
Boil white ppt. White ppt. - (Zn ) If Group IV is absent, to the O.S. add solid NH4Cl, NH4OH and
Dissolve the black ppt. in minimum 3+
with distilled White ppt. - (Al ) 2+ 2+
water and quantity of 50% HNO3. To one part of Black ppt. - (Ni and Co ) (NH4)2CO3 solution.
Confirmation of (Fe3+)
divide the 2+
Dissolve the brown ppt. Flesh coloured ppt. - (Mn )
solution into the above solution add. dil. H2SO4
in dil. HCl and divide the 2+ 2+ 2+ 2+ If Group V is absent
two parts. and alcohol. If a white ppt. is formed Confirmation of Zn White ppt. (Ba , Sr , Ca )
2+ solution into two parts. 2+
(i) Add KI solution Pb (i) is
is indicated. If no white ppt. To one part of solution Dissolve a part of white ppt. in dil. HCl and divide the solution in two Dissolve a part of white ppt. in dil. acetic test for Mg .
to one part of add pot. ferrocyanide parts. (i) To the O.S. add a
above formed, add excess NH4OH to the acid. Boil off CO2.
solution. A prussion (i) To one part of solution add. pot. ferrocynaide solution -
solution. second part of the solution - Blue (i) To one part of the above solution, add pinch of NH4Cl, a few
blue colour or ppt. Bluish white ppt.
Yellow ppt. 2+ To second part of (ii) To second part of solution add NaOH solution. White ppt. K2CrO4 solution. Yellow ppt. Confirms groups of NH4OH
2+ coloured solution indicates Cu (ii)
.
confirms Pb . 2+ solution add. pot. soluble in excess. 2+ and excess of amm.
Confirmation of Cu Ba .
sulphocyanide solution. Confirmation of Ni2+ and Co2+ phosphate solution -
(ii) Add K2CrO4 2+ 2+ 2+ 2+
A blood red colouration. (ii) If Ba is absent, then to the second part
(i) Add excess of NH4OH solution to If the ppt. obtained is black Ni or Co is indicated. Note the colour White ppt. - Mg .
solution to the 3+
original solution. Deep blue solution. Confirmation of Al 2+ of above solution add amm. sulphate (ii) Perform charcoal
second part of of the salt. If the salt is greenish - Ni is indicated and if the salt is 2+
the (ii)
above Acidify the above deep blue solution
(i) Perform charcoal cavity - solution. A white ppt. confirms Sr . cavity cobalt nitrate
solution. with dil. acetic acid. Add Pot. cobalt nitrate test with purple Co2+ is indicated. 2+ 2+ test with white ppt. -
ferrocyanide solution. Chocolate white ppt. Blue mass. (iii) If both Ba and Sr are absent, then to A pink mass.
Yellow ppt.
2+
2+
2+ (ii) Lake test. White ppt. + Confirmation of Co the third part of the above solution add +
brown ppt. confirms Cu .
confirms Pb . dil. HCl + a few drops of ammonium oxalate solution. A white Test for NH4
(i) 2+ To the salt and
blue litmus solution + (i) Take O.S. and neutralise the acid by adding NH4OH. Add a
ppt. confirms Ca .
pinch of potassium nitrite and acidify with dil. acetic acid - sodium hydroxide
NH4OH solution in Perform the flame test with a part of the solution and heat. If
Yellow ppt.
excess. A blue ppt., (ii) Perform boraxbead test with the salt. - Blue bead salt. ammonia gas evolves
suspended in a 2+ 2+ +
(i) Light green flame-Ba confirmed. NH4 is present.
colourless medium Confirmation of Ni 2+
(called a lake) (ii) Crimson red flame-Sr confirmed. Pass the gas through
(i) Take O.S. and make alkaline by adding NH4OH and then add a 2+ Nessler’s reagent. A
few drops of dimethyl glyoxime - Bright red ppt. (iii) Brick red flame-Ca confirmed. brownish ppt. or
(ii) Perform borax bead test with the salt - Brown bead in colouration is
oxidising flame and grey bead in reducing flame. obtained.
2+
Confirmation of Mn +
Note: NH4 may be
(i) Dissolve flesh coloured ppt. in dil. HCl, boil off H 2S, add NaOH tested in the
and Br2 water. - White ppt. turning grey. beginning of analysis
of basic radicals as
(ii) Perform borax bead test with group ppt. - Pink bead in
zero group.
oxidising flame and colourless in reducing flame.