You are on page 1of 95

Welcome to

Salt Analysis
Chemical Analysis

Qualitative
The resolution of a
chemical compound into
its proximate or ultimate Chemical
parts to determine its
Analysis
elements

Quantitative
Qualitative Analysis

Finding out the nature of the


substance and identify its
constituents

Qualitative Analysis of Inorganic Salts:

Identification of
cations and anions
present in salt or mixture of
salts
Qualitative Analysis of Inorganic Salts

Part contributed Part contributed


by a base by an acid
Identification of
cations and anions
present in salt or mixture of Acidic radicals
Basic radicals
salts
Qualitative Analysis of Inorganic Salts

Example

CuSO4
Qualitative analysis is
carried out through the
Cu2+ SO42─ reactions that are easily
Cation Anion perceptible to our
senses.

Basic Radical Acidic Radical Sight, smell


and more
Reactions

01 Formation of precipitate

02 Change in colour

03 Evolution of gas
Steps In Salt Analysis

Preliminary examination of solid


Step 1 salt and its solution

Step 2 Determination of anions by


wet test and confirmatory test

Carried out in solution

Determination of cations by
Step 3
wet test and confirmatory test

Carried out in solution


Preliminary Tests

These tests involve noting of


general appearances and
physical properties

Colour, smell
and Solubility
They are usually performed
within 10-15 minutes
These tests
are not conclusive but sometimes
provide important clue.
Analysis of Anions

Based on mixing with acid, anions


are classified as:

Group A Group B Group C

Produces Produces Does not


vapour/gas on vapour/gas on produce any
mixing with dil. mixing with vapour/gas with
H2SO4/HCl conc. H2SO4/HCl any of them
− −
2− 2− E.g. (NO3 ), (Cl ), 2−
E.g. (CO3 ), (S ) − − E.g. (SO4 )
(Br ),(l )
Analysis of Anions

Confirmatory (wet)
tests
for anions are performed
either by using water Water extract is
extract when salt is made by dissolving
soluble in water or by salt in water.
using sodium
carbonate extract when
salt is insoluble in
water.
Sodium Carbonate Extract

Preparation Take 1 g of salt in a porcelain dish


or boiling tube. Mix about 3 g of
solid sodium carbonate and add
15 mL of distilled water to it .

Stir and boil the content for about


10 minutes. Once it cools, filter
and collect the filtrate in a test
tube.
Confirmation Test for CO32 ─

Confirmation of CO32−is done Take 0.1 g of salt in a test tube, and


01 add dilute sulphuric acid.
by using aqueous solution of
the salt or by using solid salt
as such.
CO2 gas is evolved with brisk effervescence,
which turns lime water milky.
02

Sodium carbonate
extract contains On passing the gas for some more
carbonate ions 03 time, milkiness disappears.
Confirmation Test for CO32 ─

The evolution of colourless and odourless


2−
gas indicates the presence of CO3

Na2CO3 + H2SO4 Na2SO4 + H2O + CO2

Ca(OH)2 + CO2 CaCO3 + H2O

Milky

CaCO3 + CO2 + H2O Ca(HCO3)2

Soluble in water
Note!!

Soluble bicarbonates give


white precipitate with
MgSO4(aq)/MgCl2(aq) only
on heating.


Mg2+ + 2HCO3 Mg(HCO3)2
∆ MgCO3 + H2O + CO2
Confirmatory test for S2-

With warm dilute H2SO4,


sulphide gives hydrogen sulphide
gas which smells like rotten eggs.

Sulphide test is also


done by taking water
Smells like rotten eggs.
extract and sodium
carbonate extract.
Na2 S + H2SO4 Na2SO4 + H2S
Confirmatory test for S2-

A piece of filter paper dipped in


lead acetate solution turns black
on exposure to the gas due to the
formation of lead sulphide which
is black in colour.

(CH3COO)2Pb + H2S PbS + 2CH3COOH

Lead sulphide
Black colour
Confirmatory Test of S2−

Take 1 mL of water extract and Sodium


nitroprusside
make it alkaline by adding
NH4OH or Na2CO3 extract
Na2S + Na2[Fe(CN)5NO]
Red

Add a drop of sodium


nitroprusside solution Na4[Fe(CN)5NOS]
Purple

Confirms the
presence of
sulphide ion
Purple or violet colour appears
Nitrate Ion (NO−3 )

If on heating, the salt with


conc. H2SO4 light brown
fumes are evolved

2NO3- + 2H2SO4 4NO2 + 2SO42- + 2H2O + O2

Reddish Brown

On addition of small quantity of Cu turnings (i.e.,


small pieces of copper) solution turns blue due
to the formation of copper sulphate.
Confirmatory Test of Nitrate Ion (NO3− )

Brown ring test

When a freshly prepared saturated solution of iron (II)


sulphate is added to nitrate solution and then
concentrated H2SO4 is added slowly from side of the
test tube

A brown ring is obtained at the


junction of two layers
Confirmatory Test of Nitrate Ion (NO3− )

NaNO3 + H2SO4 NaHSO4 + HNO3


Reaction

6FeSO4 + 3H2SO4 + 2HNO3 3Fe2(SO4)3 + 4H2O + 2NO

FeSO4 + NO + 5H2O [Fe(H2O)5(NO)]SO4


Pentaaquanitrosoniumiron (I)
sulphate
Brown colour
Confirmatory test for SO42-

Aqueous solution or sodium


1 carbonate extract of the salt is
acidified with acetic acid.

Addition of barium chloride Reaction


gives a white precipitate
of barium sulphate.
Na2SO4 + BaCl2 BaSO4 + 2NaCl

BaSO4 is insoluble in conc. HCl Barium sulphate


or conc. HNO3. (white precipitate)
Confirmatory test for SO42-

2 Sulphate ions give white


precipitate of lead sulphate when
aqueous solution or sodium
carbonate extract is neutralised
with acetic acid and treated with
lead acetate solution.

Reaction

Na2SO4 + (CH3COO)2Pb PbSO4 + 2CH3COONa

Lead sulphate
(white precipitate)
Confirmatory Test of Cl−

On treatment with warm conc. H2SO4,


colourless pungent smelling gas (HCl) is NaCl + H2SO4 NaHSO4 + HCl
evolved.

It gives fumes of NH4Cl when


aq. ammonia solution is brought NH4OH + HCl NH4Cl + H2O
in contact with evolving gas
Dense
White
fumes
Confirmatory Test of Cl−

1 Silver nitrate test White precipitate is soluble


in aqueous ammonia and
precipitate reappears with HNO3.
Cl– + Ag+ AgCl
(White ppt)
From AgNO3 Add aqueous ammonia

AgCl + 2NH4OH [Ag(NH3)2]Cl + 2H2O


(soluble)
+
[Ag(NH3)2]Cl + 2H+ AgCl + 2NH4
(White ppt)
From HNO3
Confirmatory Test of Cl−

2 chromyl chloride test 4NaCl + K2Cr2O7 + 6H2SO4

Mix a small amount of salt and an 2KHSO4 + 2CrO2Cl2 + 4NaHSO4 + 3H2O


equal amount of solid K2Cr2O7 in a test
tube and add conc. H2SO4 to it. Chromyl chloride

CrO2Cl2 + 4NaOH
Heat the test tube and pass the evolved
gas through sodium hydroxide solution.
Na2CrO4 + 2NaCl + 2H2O

If a yellow solution is obtained,


then divide it into two parts.
Confirmatory Test of Cl−

Acidify the first part with acetic acid


and then add lead acetate solution.

The formation of yellow precipitate of


lead chromate confirms the presence
of chloride ions.

(CH3COO)2Pb + Na2CrO4 PbCrO4 + 2CH3COONa


Sodium Lead chromate
chromate (Yellow precipitate)
Confirmatory Test of Br−
1
Heating salt with conc. H2SO4 results in Indicates the presence
the evolution of reddish brown fumes −
of Br ions.
of bromine in excess.

2NaBr + 2H2SO4 Br2 + SO2 + Na2SO4 + 2H2O


Reddish Brown

Fumes are intensified by the Bromine vapours turn starch


addition of MnO2. paper yellow.

2NaBr + MnO2 + 2H2SO4 Na2SO4 + MnSO4 + 2H2O + Br2

Fumes of bromine intensifies


Confirmatory Test of Br−

Add 1 mL of CCl4/CHCl3 and excess of


2 freshly prepared chlorine water
dropwise to salt in water or Na2CO3
extract neutralised with dil. HCl.

2NaBr + Cl2 2NaCl + Br2

Due to dissolution of bromine, the orange


brown coloration in the organic layer,
confirms the presence of bromide ions.
Confirmatory Test of Br−

Acidify the sodium carbonate extract of


3 the salt with dil. HNO3 . Add silver nitrate
(AgNO3) solution and shake the test
tube.

A pale yellow precipitate is obtained


that dissolves in ammonium hydroxide
with difficulty

NaBr + AgNO3 NaNO3 + AgBr

Silver bromide
Pale yellow
precipitate

Test of I

On dissolving in H2SO4, violet Conc. H2SO4+ KI KHSO4 + SO2 + I2


vapours appears, which
turns starch paper blue.
Violet Fumes

Fumes become dense on adding


MnO2 to the reaction mixture. I2+ Starch Deep Blue

Starch Iodine Complex

The above observation means it


may be I-

Confirmatory Test of I

Acidify sodium carbonate extract


1 of the salt with dil. HNO3 and add
AgNO3 solution.

Appearance of yellow precipitate


insoluble in excess NH4OH

Confirms the presence


of iodide ions

NaI + AgNO3 NaNO3 + Agl

Silver iodide
Yellow precipitate

Confirmatory Test of I

Add 1 mL of CHCl3 or CCl4 and chlorine


water in excess to the salt solution in water
2
or sodium carbonate extract neutralised
with dil. HCl

shake the test tube


vigorously.

Violet colouration in organic layer


confirms the presence of iodide ions

NaI + Cl2 NaCl + l2


Determination of cations by wet
test and confirmatory test
Classification of cations in groups and their reagents

Group Cations Group reagent

Zero NH4+ None

Group – I Ag+, Pb2+, Hg22+ Dilute HCl

Cd2+, Sn2+, Sb3+, Pb2+,


H2S gas in the
Group – II Hg2+, Bi3+, Cu2+, As3+,
presence of dil. HCl
Sn4+

NH4OH in the
Group –III Al3+, Fe3+, Cr3+
presence of NH4Cl
Classification of cations in groups and their reagents

Group Cations Group reagent

H2S in the presence of


Group - IV Zn2+, Mn2+, Co2+, Ni2+
NH4OH

(NH4)2CO3 in the
Group – V Ba2+, Sr2+, Ca2+
presence of NH4OH

Group – VI Mg2+ None


Steps Involved in Examination of Cations

Preliminary examination
01 of the salt for identification
of cation

Wet tests for the


confirmation of cations 02
Preliminary Examination

Colour test

Identification of
Dry heating test
cations by

Flame Test
Colour Test

Cations
Colour
indicated

Light green,
Fe2+, Fe3+
yellow, brown

Blue Cu2+

Bright Green Ni2+

Blue, red, violet,


Co2+
pink

Light Pink Mn2+


Dry Heating Test

Take about 0.1 g of the dry salt in


a clean and dry test tube.

Heat the above test tube


for about one minute
and observe the colour
of the residue when it is hot
and also when it gets cold.
Dry Heating Test

Colour Colour
Inferences
when Cold when hot

Blue White Cu2+

Dirty white
Green Fe2+
or yellow

White Yellow Zn2+

Pink Blue Co2+


Flame Test

Colour of the
Colour of the
flame observed
flame observed Inference
through blue
by naked eye
glass

Same colour as
Green flame with
observed without Cu2+
blue centre
glass

Crimson red Purple Sr2+

Apple green Bluish green Ba2+

Brick red Green Ca2+


Wet Tests

The first essential step is to


prepare a clear and
transparent solution of salt.

Original solution(O.S.)
Analysis of zero group cation

Analysis of
+
NH4 ion
Take 0.1 g of salt in a test tube and
add 1-2 mL of NaOH solution to it
and heat.

Smell of Ammonia.

Indicates the presence


of ammonium ions
Confirmatory Test for NH4+ Ion

Ammonia gas evolved by the


action of sodium hydroxide,

And gives ammonium chloride


when reacts with HCl

Dense white fumes

(NH4)2SO4 + 2NaOH Na2SO4 + 2NH3 + 2H2O

NH3 + HCl NH4Cl


White fumes
Confirmatory test for NH4+ ion

Bring glass rod dipped in HCl near to


the mouth of test tube. White fumes
(of NH4Cl) are observed
K2[Hgl4]

Pass this gas through Nessler’s


reagent

Brown precipitate is obtained


Confirmatory test for NH4+ ion

On passing the gas through Nessler’s reagent,


a brown colouration or a precipitate of basic
mercury(II) amido-iodine is formed.

2K2Hgl4 + NH3 + 3KOH HgO.Hg(NH2)l + 7Kl + 2H2O

Basic mercury (II) amido-iodine


(Brown precipitate)
For the analysis of cations belonging to groups I-VI, the cations are
precipitated from original solution by using the group reagents

Original solution
(O.S.)
Dil. HCl

Precipitate, If no precipitate
Group I is formed

(Pb2+, Hg2+ , Ag+) as Pass H2S gas


2
chloride

If no precipitate, take
Precipitate, Group II
original solution

(Hg2+, Pb2+, Bi3+, Cu2+, Cd2+) as


sulphide
Heat (O.S.) with conc. add solid NH4Cl + NH4OH
HNO3, cool solution in excess

Precipitate, Group III If no precipitate


(Al3+, Cr3+, Fe3+) as Pass H2S gas
hydroxides

If no precipitate, take
Precipitate, Group IV
original solution
(Zn2+, Mn2+, Ni2+, Add NH4OH and
Co2+) as sulphides solid (NH4)2CO3

Precipitate, Group V If no precipitate,


take original
(Ba2+, Sr2+, Ca2+) solution to test
as carbonates Group VI, Mg2+
Confirmatory Tests of Pb2+ ions

Test-1 On adding potassium iodide (KI) to the O.S., a


yellow precipitate of lead iodide is obtained
which confirms the presence of Pb2+ ions

PbCl2 + 2KI PbI2 + 2KCl


(Hot O.S.) Yellow
precipitate

Soluble in boiling water and


reappears on cooling as
shining crystals
Confirmatory Tests of Pb2+ ions

On addition of potassium chromate (K2CrO4)


Test-2
solution a yellow precipitate of lead
chromate is obtained. This confirms
the presence of Pb2+ ions.

PbCl2 + K2CrO4 PbCrO4 + 2KCl


(Hot O.S.) Lead chromate
(Yellow
precipitate)
Confirmatory Tests of Pb2+ ions

Reaction
The yellow precipitate (PbCrO4)
is soluble in hot NaOH solution

PbCrO4 + 4NaOH ⇌ Na2[Pb(OH)4] + Na2CrO4


Sodium tetra
hydroxoplumbate (II)
Confirmatory Tests of Pb2+ ions

Test-3 A white precipitate of lead sulphate


(PbSO4) is formed on addition of alcohol
followed by dil. H2SO4

PbCl2 + H2SO4 PbSO4 + 2HCl


Lead sulphate
(white precipitate)
Confirmatory Tests of Hg22+ Ions

Dilute HCl Solution:

White precipitate is formed


in cold solution

Hg22+ + 2HCl Hg2Cl2 + 2H+


White
precipitate
Confirmatory Tests of Hg22+ Ions

Ammonia A mixture of mercury metal (black


solution: precipitate) and basic mercury (II)
amido chloride (white precipitate) is
formed

2Hg2Cl2+ 4NH4OH HgO.Hg(NH2)Cl + Hg + 3NH4Cl +3H2O

Black

Dissolution of white precipitate


(Hg2Cl2) in aqua regia

3Hg2Cl2+ 2HNO3+6HCl 6HgCl2+ 2NO + 4H2O


Confirmatory Tests of Hg22+ Ions

Potassium iodide
solution : With Potassium iodide
solution it forms green
precipitate

Green precipitate in excess


of reagent undergoes
disproportionation reaction

_ 2 _
Hg2I2 (s) + 2I [HgI4] + Hg (Finely divided)
Confirmatory Tests of Hg22+ Ions

Boiling the mercury (I) iodide precipitate


with water, disproportionation takes
place and a mixture of red mercury (II)
iodide precipitate and black
mercury is formed.

Hg2I2 (s) HgI2 + Hg


Confirmatory Tests of Hg22+ Ions

Potassium chromate solution :

A red crystalline precipitate is formed


which turns black when solution of
sodium hydroxide is added.

Hg22+ + CrO42─ Hg2CrO4

Hg2CrO4(s) + 2OH─ Hg2O + CrO42─ + H2O


Confirmatory Tests of Hg22+ Ions

Potassium cyanide solution:

A black precipitate of
mercury is obtained

Hg22++ 2CN─ Hg + Hg(CN)2


Analysis of Group II (Cu2+, Pb2+) Cation

If group I is absent, add excess of


water to the same test tube.

Warm the solution and pass H2S gas


for 1-2 minutes. Shake the test tube.

A precipitate appears indicates the


presence of group II cations.
Analysis of Group II (Cu2+, Pb2+) Cation

Pass more H2S gas through the


solution to ensure complete
precipitation and separate the
precipitate

Black Cu2+ or Pb2+ present


Confirmatory Test of Pb2+ Ion

Lead sulphide precipitate dissolves


in dil. HNO3

On adding dil. H2SO4 and few drops


of alcohol to this solution a white
precipitate of lead sulphate appears Indicates the presence
of lead ions
3PbS + 8HNO3 3Pb(NO3)2 + 2NO + 3S + 4H2O

Pb(NO3)2 + H2SO4 PbSO4 + 2HNO3

Lead sulphate
(White precipitate)
Test for Lead Ion (Pb2+)

The white precipitate dissolves in


ammonium acetate solution on
boiling.

When this solution is acidified with


acetic acid and potassium chromate
solution is added, a yellow precipitate
of PbCrO4 is formed.

On adding potassium iodide


solution, a yellow precipitate
of lead iodide is formed.
Test for Lead ion (Pb2+)

PbSO4 + 4CH3COONH4 (NH4)2[Pb(CH3COO)4] + (NH4)2SO4

Ammonium
tetraacetoplumbate (II)

2−
Pb2+ + CrO4 PbCrO4

Lead chromate
(Yellow precipitate)

Pb2+ + 2I Pbl2

Lead iodide
(Yellow precipitate)
Test for Copper ion (Cu2+)

On heating reaction mixture


for long time, sulphur is
Copper sulphide dissolves in HNO3
oxidised to sulphate and
due to the formation of copper nitrate
copper sulphate is formed and
solution turns blue

3CuS + 8HNO3 3Cu(NO3)2 + 2NO + 3S + 4H2O


A small amount of NH4OH
precipitates basic copper
sulphate

Which is soluble in excess of


NH4OH due to the formation of
tetramminecopper (II) complex
Test for Copper ion (Cu2+)

Reaction S + 2HNO3 H2SO4 + 2NO

2− +
2Cu2+ + SO4 + 2NH3 + 2H2O Cu(OH)2.CuSO4 + 2NH4
2−
Cu(OH)2.CuSO4 + 8NH3 2[Cu(NH3)4]2+ + 2OH− + SO4
Tetraamminecopper (II) sulphate
(Deep blue)
Test for Copper ion (Cu2+)

The blue solution on acidification with acetic


acid and then adding potassium ferrocyanide
K4[Fe(CN)6] solution
gives a chocolate colouration due to formation
of copper ferrocyanide Cu2[Fe(CN)6]

Reaction
[Cu(NH3)4]SO4 + 4CH3COOH CuSO4 + 4CH3COONH4

2CuSO4 + K4[Fe(CN)6] Cu2[Fe(CN)6] + 2K2SO4


Potassium Copper
hexacyanoferrate (II) hexacyanoferrate (II)
(Chocolate brown
precipitate)
Confirmatory Tests For Cu2+ Ions

Sodium hydroxide in cold solution

A white precipitate is formed which


is soluble in excess of the reagent


Cu2+ + 2OH Cu(OH)2

Heat
Cu(OH)2(s) CuO (red) + H2O
Analysis of Group III Cations

Group III Cations


Al3+,Fe3+ If group II is absent, take original
solution and add 2-3 drops of conc.
HNO3

Heat the solution for few minutes

After cooling add a small amount of


solid NH4Cl and an excess of NH4OH
solution till it smells ammonia
Analysis of Group III Cations

Shake the test tube

Presence of brown or
white precipitate

Indicates the presence


group III cations
Analysis of Group III Cations

Observe the colour and the


nature of the precipitate.

A gelatinous white precipitate


indicates the presence of Al3+ ions.

A brown precipitate indicates the


presence of Fe3+ ions.
Tests for Group III

Original Solution

Add 2-3 drops of conc. HNO3, heat, add small


amount of NH4Cl(s) and excess of NH4OH
Brown/gelatinous
white precipitate

Group III present

Gelatinous white Brown


Precipitate Precipitate

Al3+ Present Fe3+ Present


Analysis of Group III Cations

Reaction
Third group cations are
precipitated
When original solution is heated with as their hydroxides
conc. HNO3, ferrous ions are oxidised
to ferric ions.

Which dissolve in dilute


hydrochloric acid due to the
[O]
FeCl2 FeCl3 formation of corresponding
chlorides
Test for AI3+ ions

When the solution containing aluminium


Test-1 chloride is treated
with sodium hydroxide,

AlCl3 + 3NaOH Al(OH)3 + 3NaCl

White gelatinous precipitate of aluminium hydroxide is


formed which is soluble in excess of sodium hydroxide solution

Al(OH)3 (s) + NaOH NaAlO2 + 2H2O Due to the


formation of
White Sodium sodium meta
meta aluminate
gelatinous
precipitate aluminate
Test for AI3+ ions

Test-2 When blue litmus is added to the


solution, a red colouration is obtained
due to acidic nature of the solution.

On addition of NH4OH solution drop by


drop, the solution becomes alkaline and
aluminium hydroxide is precipitated.
Test for AI3+ ions

Aluminium hydroxide adsorbs blue


Test-2 colour from the solution and forms
insoluble adsorption complex named
‘lake’

Thus, a blue mass floating in the


colourless solution is obtained.

Lake test
Test for Fe3+ ions

Reddish brown precipitate of ferric When the solution containing ferric


hydroxide dissolves in hydrochloric chloride is treated with potassium
acid and ferric chloride is formed ferrocyanide solution, a blue
precipitate/colouration is obtained.

Reaction
The colour of the precipitate is
Fe(OH)3 + 3HCl FeCl3 + 3H2O Prussian blue. It is ferric ferrocyanide
Test for Fe3+ ions

Reaction 4FeCl3 + 3K4[Fe(CN)6] Fe4[Fe(CN)6]3 + 12KCl

Potassium Prussian Blue


ferrocyanide Precipitate

If potassium ferrocyanide is added in


excess, then a product of composition
KFe[Fe(CN)6] is formed.

This tends to form a colloidal solution


(soluble Prussian blue) and cannot be
filtered.
Test for Fe3+ ions

Reaction FeCl3 + K4[Fe(CN)6] KFe[Fe(CN)6] + 3KCl

Soluble prussian blue

To the second part of the solution,


add potassium thiocyanate Fe3+ + 3SCN− [Fe(SCN)3]
(potassium sulphocyanide) solution.
Blood red colour

The appearance of a blood red


colouration confirms the presence
of Fe3+ ions.
Analysis of Group IV Cations

Group IV Cations
Ni2+, Zn2+
If group-III is absent, pass H2S gas
in the solution of group
III for few minutes

If a precipitate appears (white, black


or flesh coloured), this indicates the
presence of group IV cations
Analysis of Group IV Cations

Fourth group cations are precipitated


as their sulphides.

Observe the colour of precipitate

White colour Black colour

Presence of Presence of
Zn2+ ions Ni2+ ions
Analysis of Group IV Cations

Tests for Zinc ions


(Zn2+)

Zinc sulphide dissolves in hydrochloric


acid to form zinc chloride

Reaction

ZnS + 2HCl ZnCl2 + H2S


Test For Zn2+ Ions

On addition of sodium hydroxide ZnCl2 + 2NaOH Zn(OH)2 + 2NaCl


solution, it gives white precipitate
of zinc hydroxide

Which is soluble in excess NaOH


Zn(OH)2 + 2NaOH Na2ZnO2 + 2H2O
solution on heating.
Sodium zincate
(Soluble)
Confirms the
presence of Zn2+ ions
Test For Zn2+ Ions

When potassium ferrocyanide


K4[Fe(CN)6] solution is added to the
solution after neutralisation by NH4OH
solution

A white or bluish white precipitate of


zinc ferrocyanide appears.

Reaction

2 ZnCl2 + K4[Fe(CN)6] Zn2[Fe(CN)6] + 4KCl

Zinc ferrocyanide
(white-bluish ppt)
Analysis of Group IV Cations

Tests for Nickel ions (Ni2+)

3NiS + 2HNO3 + 6HCl 3NiCl2 + 2NO + 3S + 4H2O

The black precipitate of nickel


sulphide dissolves in aqua regia
Test For Ni2+ Ions

After treatment with aqua regia,


nickel chloride is obtained,
which is soluble in water

When dimethyl glyoxime is added


to the aqueous solution of nickel
chloride made alkaline by
adding NH4OH solution

A brilliant red
precipitate is obtained
Test For Ni2+ Ions

Reaction NiCl2 + 2NH4OH + 2

2+
+ 2NH4Cl + 2H2O

Complex of red colour


(stable form of complex)
Analysis of Group V Cations

Group V Cations
Ba2+, Ca2+
Take original solution and add small
amount of solid NH4Cl and an
excess of NH4OH solution followed by
solid ammonium carbonate (NH4)2CO3

White precipitate indicates the


presence of group V cations
Analysis of Group V Cations

Dissolve the white precipitate by


boiling with dilute acetic acid

And divide the solution into 2 parts,


one each for Ba2+ and Ca2+ ions

Preserve a small amount of


precipitate for flame test
Test For Ba2+ Ions

Potassium chromate (K2CrO4) solution


gives a yellow precipitate of barium
chromate when the solution of fifth group
precipitate in acetic acid is treated with it

BaCO3 + 2CH3COOH (CH3COO)2Ba + H2O + CO2

(CH3COO)2Ba + K2CrO4 BaCrO4 + 2CH3COOK

Barium chromate
(yellow precipitate)
Flame Test For Ba2+ Ions

A grassy green colour


of the flame confirms the
presence of Ba2+ ions.
Test for Ca2+ Ions

Solution of the fifth group precipitate in


acetic acid gives a white precipitate
with ammonium oxalate solution.

CaCO3 + 2CH3COOH (CH3COO)2Ca + H2O + CO2

(CH3COO)2Ca + (NH4)2C2O4 (COO)2Ca + 2CH3COONH4

Ammonium Calcium oxalate


oxalate (White precipitate)
Flame Test for Ca2+ Ions

Perform
the flame test.
. Calcium imparts brick
red colour to the
flame, which looks
greenish-yellow
through
blue glass.
Analysis of Group VI Cation (Mg2+)

If group V is absent, the solution may


contain magnesium carbonate, which is
soluble in water in the presence of
ammonium salts because the equilibrium is
shifted towards
the right-hand side.

2−
NH+

4 + CO3 NH3 + HCO3
Test for Mg2+ Ions

The concentration of carbonate ions


required to produce a precipitate
is not attained.

Indicates the
When disodium hydrogenphosphate
presence of
solution is added and the inner walls of
Mg2+ ions
the test tube are scratched with
a glass rod,

A white crystalline precipitate of


magnesium ammonium phosphate is
formed.
Test for Mg2+ Ions

Reaction

Mg2+ + Na2HPO4 Mg(NH4)PO4 + NH4OH + 2Na+ + H2O

Magnesium ammonium
phosphate (White precipitate)

You might also like