Sri Chaitanya Educational Institutions, India

Chemistry Lab Manual

Systematic Qualitative Analysis of Simple Inorganic Salt
Qualitative analysis of simple inorganic salt is carried out under Three steps:
I. Preliminary Tests
II. Detection of Anion (negative radical, acid radical)
III. Detection of Cation (positive radical, basic radical)
I. Preliminary Tests

Test Observation Inference

Soluble Salts containing
1. Appearance
Crystaline Cl − , Br − , NO3− , SO42− may
(Physical State)
be present
Insoulble salt containing
Amorphous
CO32− may be present

2. Colour Pale Pink Mn 2+ may be present

Colourless (White) Mn 2+ may be absent

Salt containing anion like

3. Solubility Test
Soluble Cl − , Br − , NO3− , SO42− may
Salt + Water
be present
2−
Salt containing anion CO3
Insoluble
may be present

II. Detection of Anion (negative radical, acid radical)

Test Observation Inference
2−
Grou 1. Brisk effervescence. Colourless gas is Group I radical CO3
Salt + dil. HCl or dil.H 2 SO4 evolved may be present
2−
Group I radical is CO3
No effervescence
absent
Group 2. Colourless gas which gives thick −
Salt + conc. H 2 SO4 fumes with a glass rod dipped in Group II radical Cl
NH 4OH soln may be present

Reddish brown vapours in cold

Group II radical Br −
may be present
−
Reddish brown vapours on heating. Group II radical NO3
Intensity of colour increases with may be present
Page 1
Sri Chaitanya Educational Institutions, India
addition of pieces of ' Cu ' turnings

−
Group II radical is Cl
If No Particular gas is evolved
Cl − , Br − , NO3− absent
Group 3. White pot insoluble even in 2−
Group III radical SO4
Salt.so ln + BaCl2 so ln hot. dil. HCl may be present
Confirmatory Test for Anions
2−
Group1 – Radical : CO3
2−
C.T for CO3 :
Salt + dilHCl or
dil H 2 SO4 , CO2 gas is liberated
CO32− is present and
with brisk effervescence . The Lime water turns milky
confirmed
liberated gas is passed through
freshly prepared lime water
− − −
Group II Radical : Cl , Br , NO3

C.T for Cl − : White curdy ppt easily soluble in Cl − is present and

1. Silver nitrate Test: excess of NH 4OH confirmed
Salt soln + AgNO3 soln
2. Chromyl Chloride Test:
Salt + equal amount of K 2Cr2O7
crystals + a few drops of
conc.H 2 SO4 . Heat the mixture.
Yellow ppt
Cl − is present and
The red vapours containing confirmed
1 − 2cm NaOH solution. Then
3

add acetic acid and lead acetate

solution.
C.T for Br − (Glouble Test)
5 drops of salt soln + 3 drops of An orange or reddish brown globule in Br − is present and
CCl4 or CHCl3 + 5 drops of the organic layer confirmed
chlorine water shake well.
C.T for NO3− (Brown ring Test):
Salt soln ( 5 drops) + 5 drops
freshly prepared ferrous sulphate
A brown ring is formed at the junction NO3− is present and
solution + 2-3 drops of conc.
of two layers confirmed
H 2 SO4 cool the mixture along the
wall of the test tube (without
disturbing the contents)

Page 2
Sri Chaitanya Educational Institutions, India
2−
C.T for SO4 White ppt which is soluble in hot SO42− is present and
Salt soln + lead acetate soln (5 ammonium acetate confirmed
drops)

III. Detection of cation (positive radical, basic radical)

Preparation of Original Solution (O.S)
Suppose salt is soluble in water, dissolve 0.5 g of salt in 10cm3 of distilled water. This solution called O
S Suppose the salt is insoluble in water, dissolve 0 5 g of salt in minimum quantity of dil HCl . Then
make the volume upto 10 cm3 by adding distilled water. This solution is called O S.
Test Observation Inference
Group 0 test: Colourless gas liberated Group 0 radical is present
Salt + dil. NaOH a) Gives white thick fumes with ( NH )
+
4

glass rod dipped in dil.HCl soln

b) Turns moist red litmus paper
into blue
c) Possesses smell of ammonia

No action (no smell of ammonia)

Group 0 radical ( NH 4+ ) is absent

Group1test: No PPT Group 1 radical Pb +2 is absent

O S + dil HCl
White ppt Group 1 radical is present Pb +2
Group 2 No PPT Group II radicals Pb+2 , Cu +2 is
O S + dil HCl (warm) + H2S absent
Black ppt Group II radicals Cu +2 present

Group 3 No PPT Group III is absent Al +3

O S + NH4Cl (excess) +
NH4OH(2 or 3 drops)
White gelatinous PPT Group III present Al +3
Group 4 No PPT (
Group IV radical Zn 2+ , Mn 2+ )
O S + NH 4Cl (excess) +
is absent
NH 4OH + H 2 S

Page 3
Sri Chaitanya Educational Institutions, India
White ppt or pale pink ppt Group IV radical is present

( Zn 2+
, Mn 2+ )

Group 5 No PPT Group V radicals

O S + NH 4Cl (excess) + ( Ba 2+
, Sr 2+ , Ca 2+ ) absent
NH 4OH + ( NH 4 )2 CO3
White PPT Group V radical

( Ba 2+
, Sr 2+ , Ca 2+ )
present.
Group 6 No PPT Group 6 radical Mg 2+ is ( )
O S + NH 4Cl +
absent
NH 4OH + Na2 HPO4
White PPT Group VI radical Mg 2+ is ( )
present

(
Analysis of Group Zero Radical NH 4+ )
Test Observation Inference
O S + Nessler’s Reagent Reddish brown PPT NH 4+ is present and
confirmed
Analysis of Group I Pb +2
Test Observation Inference
O S + KI Yellow PPt Pb +2 confirmed

O S + K 2CrO4 Yellow PPt Pb +2 confirmed

Analysis of Group II Pb +2
Test Observation Inference
O S + KI Yellow PPt Pb +2 confirmed

O S + K 2CrO4 Yellow PPt Pb +2 confirmed

Analysis of Group II Cu +2
Test Observation Inference
O S + K 2 Fe(CN )6 Brick red ppt Cu +2 is confirmed

O S + KI Brown ppt Cu +2 is confirmed

Page 4
Sri Chaitanya Educational Institutions, India
Analysis of Group III Al 3+ ( )
Test Observation Inference
O S + 1- 2 drops of dil NaOH soln White gelatinous PPT soluble in Al 3+ is present and
excess of NaOH confirmed

(
Analysis of Group IV Zn 2+ , Mn 2+ )
Test Observation Inference
O S + NH 4Cl + NH 4OH + H 2 S a) White PPT Zn2+ is present
b) Flesh colour PPT
Mn2+ is present

C.T for Zn2+ White PPT soluble in excesss of Zn2+ is present and
NaOH solution. confirmed
O S + 1 – 2 drops of NaOH soln

C.T for Mn2+ White PPT turns brown on exposure Mn2+ is present and
to air. confirmed
O S + 1 – 2 drops of NaOH soln

(
Analysis of Group V Ba 2+ , Sr 2+ , Ca 2+ )
Test Observation Inference

C.T for Ba 2+
Yellow PPT which is insoluble in
1) O S + K 2CrO4 soln
acetic acid Ba2+ is present & Confirmed

2) Flame test:
Apple green
A paste of the given salt is
prepared with few drops of
Conc.Hcl and it is exposed to the
colourless flame through Pt wire.

C.T for Sr 2+

1) O S + ( NH 4 )2 SO4 soln
white PPT which is soluble in
Sr 2+ is present and
acetic acid
confirmed
2) Flame test
A paste of the given salt is prepared with few Crimson red
drops of Conc.Hcl and it is exposed to the

Page 5
Sri Chaitanya Educational Institutions, India
colourless flame through Pt wire.

C.T forCa+2

1) O S + Ammonium oxalate White PPT insoluble in acetic acid

Ca2+ is present and

2) Flame test confirmed
A paste of the given salt is Brick red colour
prepared with few drops of
Conc.Hcl and it is exposed to the
colourless flame through Pt wire.

Analysis of Group VI Mg 2+ ( )
Test Observation Inference
First test:
O S + NH 4Cl + White crystalline ppt.

NH 4OH + Na2 HPO4 scratch the Mg 2+ is present and confirmed

inner walls of the test tube.

White PPT soluble in excess
Second test:
of NH 4Cl
O S +1 − 2 drops of NaOH so ln
.
Report: Anion : ________
Cation :_________ Hence the given salt is___________

Page 6
Sri Chaitanya Educational Institutions, India

VOLUMETRIC ANALYSIS – I
KMnO4 vs FAS [Redox Titration]

AIM : To prepare 100mL of M/50 Ferrous Ammonium Sulphate solution. Using this solution, determine the molarity
and strength of given KMnO4 solution.

APPARATUS REQUIRED : Pipette, Conical flask, Porcelain tile, Burette, Burette stand, Test tube, etc.,

CHEMICALS REQUIRED : KMnO4 , Ferrous Ammonium Sulphate, H2SO4 and distilled water.

PRINCIPLE :

Reduction half reaction : MnO4- + 8H+ + 5e- -------> Mn2+ + 4H2O

Oxidation half reaction : Fe2+-------> Fe3+ +e-
Overall reaction : MnO4 + 8H +5 Fe2+ -------> Mn2+ + 4H2O + Fe3+
- +

Molecular form of equation : 2KMnO4 + 8H2SO4 +10 FeSO4 -------> K2SO4+ 2MnSO4 + 5 Fe2(SO4)3+ 8H2O

CALCULATION OF WEIGHT OF FAS REQUIRED :

Mass of FAS crystals x 1000 litre
Molarity of FAS solution =
GMM of FAS x 100
1/50 moles / litre = Mass of FAS crystals x 1000 litre
392 g/mole x 100
Mass of FAS crystals = 0.784 g

CALCULATION OF MOLARITY OF PREPARED FAS SOLUTION :

Weight of paper + weight of FAS crystals = 1.0576 g
Weight of paper after transferring FAS crystals = 0.2738 g
Weight of FAS crystals transferred = 0.7838 g
0.7838 x 1000
Molarity of FAS solution = 392 100
Molarity of prepared FAS solution is 0.01999 moles/ litre.

SHORT PROCEDURE :

Burette solution – KMnO4 solution

Pipette solution - FAS solution (or) Mohr’s salt solution
Indicator - Self indicator (KMnO4)
Auto- catalyst - Mn+2
Condition - Room temperature & pressure
End point - Appearance of permanent pale pink colour
Medium - Acidic ( nearly 4N H2SO4 solution)
GMM of FAS - 392 g/mole
GMM of KMnO4 -158 g/mole

TABULAR COLUMN :

S.No Volume of FAS Burette reading (mL) Volume of KMnO4 solution Concordant value (mL)
solution (mL) (mL)
Initial Final

Page 7
Sri Chaitanya Educational Institutions, India

As per law of volumetric analysis,

V1M1 = V2M2
n1 n2
V1 – Volume of KMnO4 solution
M1- Molarity of KMnO4 solution
n1- Stoichiometric co-efficient of KMnO4 as per balanced equation
V2 – Volume of FAS solution
M2- Molarity of FAS solution
n2- Stoichiometric co-efficient of FAS as per balanced equation

CALCULATION :

RESULT : For the given KMnO4 solution ,

i. Molarity is moles litre-1
ii. Strength is g/L

Page 8