You are on page 1of 50

QUANTITATIVE

ANALYSIS
VOLUMETRIC
ANALYSIS
VOLUMETRIC ANALYSIS-1
Aim:
Prepare M/50 solution of oxalic acid. Use this solution to determine
molarity and the strength of the given potassium permanganate
(KMnO4) solution.

Theory:
The quantity of oxalic acid required for the 250ml of the solution
having a molarity of 0.02M can be calculated as follows.
Molar mass of oxalic acid = 126g/mol
Molarity =mass/Molar mass x V(L)

Mass of oxalic acid required for the 250ml


=molarityxmolarmassx250/1000

=0.02x 126 x250 / 1000


=0.63g
For the preparation of 250 mL of M/50 oxalic acid solution amount
of oxalic acid required = 0.63 g

Potassium permanganate is a strong oxidising agent and in the


presence of sulphuric acid it acts as a powerful oxidising agent. In
acidic medium the oxidising ability of KMnO4 is represented by the
following equation.
In acidic solution,
MnO4– + 8H+ + 5e– → Mn2+ + 4H2O
Solution containing MnO4– ions are purple in colour and the
solution containing Mn2+ ions are colourless and hence
permanganate solution is decolourised when added to a solution of
a reducing agent. The moment there is an excess of potassium
permanganate present the solution becomes purple.
Thus KMnO4 serves as self indicator in acidic solution.
Potassium permanganate is standardised against pure oxalic acid.
It involves a redox reaction. Oxalic acid is oxidised to carbon
dioxide by KMnO4 which itself gets reduced to MnSO4. Oxalic acid
reacts with potassium permanganate in the following way.
The chemical reaction at room temperature is given below.

The ionic equation involved in the process is given below.

This titration cannot be carried out in the presence of acids like


nitric acid or hydrochloric acid because itself is an oxidising agent.
So hydrochloric acid chemically reacts with KMnO4 solution
forming chlorine which is also an oxidising agent.

Materials Required:
1. Oxalic acid
2. Potassium permanganate solution
3. 4N sulphuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing bottle
12. White tile
13. Burner
14. Wire gauze
Procedure:
(a) Preparation of 0.02M (1/50M) standard solution of oxalic
acid:

1. Weigh an empty watch glass using a chemical balance.


2. Weigh 0.63g of oxalic acid accurately in the watch glass.
3. With the help of a funnel transfer the oxalic acid into 250mL
standard flask.
4. Now wash the funnel with distilled water without removing
the funnel from the flask.
5. Make the solution up to the marked point with distilled water
and make sure the oxalic acid fully dissolved.
6. This solution is 0.02M standard solution of oxalic acid.

(b) Titration of potassium permanganate solution against


standard oxalic acid solution:

1. Rinse the burette with the potassium permanganate


solution and fill the burette with potassium permanganate
solution.
2. Fix the burette in the burette stand and place the white tile
below the burette in order to find the end point correctly.
3. Pipette out 20ml of 0.02M standard oxalic acid solution in a
conical flask.
4. Add a test tube full of sulfuric acid in order to prevent
oxidation of manganese to form manganese dioxide.
5. Heat the mixture up to 60oC before titrating with potassium
permanganate.
6. Note down the initial reading in the burette before starting
the titration.
7. The hot solution is titrated against potassium
permanganate solution and simultaneously swirl the
solution in the flask gently.
8. Initially the purple colour of KMnO4 is discharged with
oxalic acid. The appearance of permanent pink colour
reveals the end point.
9. Repeat the titration until concordant values are obtained.
10. Note down the upper meniscus on the burette readings.
Results :
1. Molarity of KMnO4 =
2. The Strength of KMnO4 =

Precautions:
1. Clean all the apparatus with distilled water before starting the
experiment and then rise with the solution to be taken in
them.
2. Rinse the pipette and burette before use.
3. Potassium permanganate is dark in colour, so always read
the upper meniscus.
4. Use dilute sulfuric acid for acidifying the potassium
permanganate.
5. Take accurate readings once it reaches the end point and
don’t go with average readings.
6. Use antiparallex card or autoparallex card while taking the
burette readings.
7. Do not use rubber cork burette as it is can be attacked by
KMnO4.
8. The strength of the unknown solution should be taken upto
two decimal places only.
VOLUMETRIC ANALYSIS-2

Aim:
Prepare M/20 solution of ferrous ammonium sulphate (Mohr’s salt).
Using this solution find out the molarity and the strength of a given
potassium permanganate solution.

Theory:
The quantity of Mohr’s salt required for the 250ml of the solution
having a molarityof 0.05M can be calculated as follows.
The molar mass of mohr’s salt = 392 g/mol
Molarity =mass/Molar mass x V(L)

Mass of mohr’s salt required for the 250ml

=molarityxmolarmassx250/1000
=0.05x 392 x250 / 1000
=4.9g
For the preparation of 250 mL of M/20 mohr’s salt solution amount
of mohr’s salt required = 4.9g

Potassium permanganate is a strong oxidant in the presence of


sulphuric acid.
Mohr salt is a double salt forming a single crystalline
structure having the formula ((NH4)2SO4. FeSO4. 6H2O. The
chemical name for Mohr’s salt is ferrous ammonium sulphate
In this titration Mohr salt acts as a reducing agent and potassium
permanganate acts as an oxidising agent. So the reaction between
Mohr’s salt and potassium permanganate is a redox reaction. In
this redox reaction, ferrous ion from Mohr’s salt gets oxidised and
pink coloured of manganese present in potassium permanganate
which is in the +7 oxidation state gets reduced to colourless
Mn2+ state.
The chemical reaction and the molecular chemical equation is
given below.

This titration is based upon oxidation-reduction titrations. When


ferrous ammonium sulphate solution is titrated against potassium
permanganate in the presence of acidic medium by sulphuric acid.
Acidic medium is necessary in order to prevent precipitation
of manganese oxide. Here KMnO4 acts as a self indicator and this
titration is called permanganate titration.

Materials Required:
1. Mohr’s salt (ferrous ammonium sulphate)
2. Potassium permanganate solution
3. Dilute sulphuric acid
4. Chemical balance
5. Burette
6. Burette stand
7. Pipette
8. Conical flask
9. Funnel
10. Measuring flask
11. Weighing bottle
12. White tile
13. Burner
14. Wire gauze
Procedure:

(a) Preparation of 0.05M standard solution of ferrous


ammonium sulfate:

1. Weigh an empty watch glass using a chemical balance.


2. Weigh accurately 4.9g of Mohr’s salt in a chemical balance.
3. With the help of a funnel transfer the Mohr’s salt into
standard flask.
4. Now wash the funnel with distilled water without removing
the funnel from the flask.
5. Make the solution up to the marked point with distilled water
and make sure the Mohr’s salt is fully dissolved.
6. This solution is 0.05N standard solution of Mohr’s salt.

(b) Titration of potassium permanganate solution


against standard ferrous ammonium sulfate (Mohr’s salt)
solution:

1. Wash and rinse the burette and pipette with distilled water
and then rinse with the corresponding solution to be filled
in them.
2. Rinse the burette with the potassium permanganate
solution and fill the burette with potassium permanganate
solution.
3. Fix the burette in the burette stand and place the white tile
below the burette in order to find the endpoint correctly.
4. Rinse the pipette and conical flask with standard ferrous
sulphate solution.
5. Pipette out 20ml of 0.05N standard Mohr’s salt solution
into the conical flask.
6. Add a test tube full of sulphuric acid in order to prevent
oxidation of manganese to form manganese dioxide.
7. Note down the initial reading in the burette before starting
the titration.
8. Now start the titration, titrate against potassium
permanganate solution and simultaneously swirl the
solution in the flask gently.
9. Initially, the purple colour of KMnO4 is discharged with
ferrous ammonium sulfate. The appearance of a
permanent pink colour reveals the endpoint.
10. Repeat the titration until concordant values are obtained.
11. Note down the upper meniscus on the burette readings.

Results:
1. Molarity of given KMnO4 solution =
2. The strength of given potassium permanganate solution =

Precautions:

1. Potassium permanganate is dark in colour, so always read


the upper meniscus.
2. Rinse the pipette and burette before use.
3. Use dilute sulfuric acid for acidifying the potassium
permanganate.
4. Clean all the apparatus with distilled water before starting the
experiment and then rinse with the solution to be taken in
them.
5. Take accurate readings once it reaches the endpoint and
doesn’t go with average readings.
6. Do not use rubber cork burette as it is can be attacked by
KMnO4.
7. Use the antiparallel card or auto parallax card while taking
the burette readings.
8. The strength of the unknown solution should be taken up to
two decimal places only.
PHYSICAL
CHEMISTRY
EXPERIMENTS
EXPERIMENT-1
EXPERIMENT-2
EXPERIMENT-3
EXPERIMENT-4
INORGANIC
CHEMISTRY
EXPERIMENTS
EXPERIMENT -1
EXPERIMENT -2
ORGANIC
CHEMISTRY
EXPERIMENTS
EXPERIMENTS-1
QUALITATIVE
ANALYSIS
SALT ANALYSIS
SALT ANALYSIS -1
I. Preliminary Examination

S.No
Experiment Observation Inference
.
1. Absence of
Copper, Iron,
Colourless
Cobalt,
Colour and appearance of the
Manganese
substance are noted
Nickel salts

2.
Action of heat:
No Absence of
A little of the salt is strongly
characteristic carbonate and
heated in a clean dry test tube
reaction acetate
3. Flame test:
Alittle of the salt is made into a
paste with few drops of conc. No Absence of
HCl. The paste is brought close to characteristic calcium, strontium
a non-luminous flame by means flame and barium
of a platinum wire

II. Systematic Analysis of Anions

S.No. Experiment Observation Inference


1. Action of Dil. HCl:
To a little of the
No characteristic Absence of carbonate
substance about 1 ml
reaction ion (CO32-)
of dil. HCl is added
slowly and heated
2. Action of dil. H2SO4:
Little of the
No characteristic
substance is rubbed Absence of acetate
reaction
with dil. H2SO4 in a ion(CH3COO-)
watch glass
3. Action with conc.
H2SO4:
Little of conc.
H2SO4 is added to a
No characteristic
little of the salt taken Absence of chloride
reaction
in a dry test tube, ion(Cl-)
warmed and then
heated strongly
4. Action with conc.
H2SO4and paper ball:
A little of salt is
strongly heated conc. No characteristic
Absence of nitrate
H2SO4 and to the reaction
ion(NO3-)
boiling solution a
paper ball is added
and again heated
5. Action with barium Presence of
chloride solution: sulphate(SO42-) ion is
A white precipitate
Barium chloride identified
insoluble in HCl is
solution is added to
obtained
little of salt solution
taken in a test tube

III. Confirmatory Tests for Anions

S.No. Experiment Observation Inference


A thick white
Sulphate: To a little of
precipitate is formed
the aqueous salt Presence of sulphate
1. which dissolved in
solution added lead confirmed
Ammonium acetate
acetate solution
solution

IV.Systematic Analysis of Cations

S.No. Experiment Observation Inference


Dil. HCl is added to a
No characteristic
1. portion of aqueous Absence of group I
reaction
salt solution cation ( lead ion,Pb2+)
No characteristic
Hydrogen sulphide is
reaction
passed through a Absence of group II
2. portion of stock cation (copper
solution to which dil. ion,Cu2+)
HCl has been added
To a little salt solution
added excess of Absence of group III
No characteristic
3. ammonium chloride cation (aluminium
reaction
ammonium hydroxide ion,Al3+)
drops to excess
Hydrogen sulphide is A white or greenish Presence of group IV
4. passed through a white precipitate is cation ( zinc ion, Zn2+)
portion of the salt formed identified
solution to which
NH4Cl and excess of
NH4OH have been
added
To a little of the salt A white precipitate
Presence of zinc ion,
solution added NaOH soluble in excess of
5. Zn2+ is confirmed.
solution drop by drop NaOH. A colourless
in excess solution is obtained
To a little of the salt
dissolved in
conc.HNO3 added a
few drops of cobalt Presence of zinc ion,
Green tinted ash is
6. nitrate and boiled. A Zn2+ is confirmed.
obtained
folded filter paper is
soaked in this
solution, dried and
burned in to ashes

RESULT:
THE GIVEN SALT IS ZINC SULPHATE (ZnSO4)
SALT ANALYSIS -2

I. Preliminary Examination

S.No. Experiment Observation Inference


1. Colour and Colourless Absence of Copper,
appearance of the Iron, Cobalt,
substance are noted Manganese Nickel
salts

2. Action of heat:
A little of the salt is No characteristic Absence of carbonate
strongly heated in a reaction and acetate
clean dry test tube
3. Flame test:
Alittle of the salt is Crimson colour Presence of
made into a paste strontium ion
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire

II. Systematic Analysis of Anions

S.No. Experiment Observation Inference


1. Action of Dil. HCl:
To a little of the
No characteristic Absence of carbonate
substance about 1 ml
reaction ion (CO32-)
of dil. HCl is added
slowly and heated
2. Action of dil. H2SO4:
Little of the
No characteristic
substance is rubbed Absence of acetate
reaction
with dil. H2SO4 in a ion(CH3COO-)
watch glass
3. Action with conc.
H2SO4: No characteristic Absence of chloride
Little of conc. reaction ion(Cl-)
H2SO4 is added to a
little of the salt taken
in a dry test tube,
warmed and then
heated strongly

4. Action with conc.


H2SO4and paper ball: Plenty of reddish Presence of nitrate
A little of salt is brown gas is evolved ion(NO3-) is identified
strongly heated conc.
H2SO4 and to the
boiling solution a
paper ball is added
and again heated
5. Action with barium No characteristic Absence of
chloride solution: reaction sulphate(SO42-) ion
Barium chloride
solution is added to
little of salt solution
taken in a test tube

III. Confirmatory Tests for Anions

S.No. Experiment Observation Inference


1. Nitrate: To an A brown ring is Presence of nitrate
aqueous salt solution formed between the ion (NO3-) is
taken in a test tube, two layers confirmed
added equal volume
of freshly prepared
ferrous sulphate and
shaken well. Then
add conc. H2SO4
carefully along the
sides of the test tube

IV.Systematic Analysis of Cations

S.No. Experiment Observation Inference


1. Dil. HCl is added to a No characteristic
portion of aqueous reaction Absence of group I
salt solution cation ( lead ion,Pb2+)
2. Hydrogen sulphide is No characteristic Absence of group II
passed through a reaction cation (copper
portion of stock ion,Cu2+)
solution to which dil.
HCl has been added
3. To a little salt solution No characteristic Absence of group III
added excess of reaction cation (aluminium
ammonium chloride ion,Al3+)
ammonium hydroxide
drops to excess
4. Hydrogen sulphide is No characteristic Absence of group IV
passed through a reaction cation ( zinc ion, Zn2+)
portion of the salt
solution to which
NH4Cl and excess of
NH4OH have been
added
5. To a little of the salt A white precipitate is Presence of group V
solution added obtained cation [barium (Ba2+),
ammonium chloride, calcium (Ca2+or
ammonium hydroxide strontium (Sr2+)] is
and excess of identified
ammonium carbonate
6. To a little of the salt No characteristic Absence of
solution added little precipitate. barium(Ba2+) ion
acetic acid and
potassium chromate
solution
7. A little of the salt A scanty white Presence of
solution is boiled with precipitate is obtained strontium(Sr2+) ion is
acetic acid and identified
ammonium sulphate
is added
8. Alittle of the salt is Crimson colour for Presence of strontium
made into a paste the flame is observed (Sr2+) ion is
with few drops of confirmed
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire

RESULT:

THE GIVEN SALT IS STRONTIUM NITRATE [Sr(NO3)2]


SALT ANALYSIS -3
I. Preliminary Examination

S.No. Experiment Observation Inference


1. Colour and Colourless Absence of Copper,
appearance of the Iron, Cobalt,
substance are noted Manganese Nickel
salts

2. Action of heat:
A little of the salt is A colourless, Presence of
strongly heated in a odourless gas is carbonate
clean dry test tube evolved which turned
lime water milky.
3. Flame test:
Alittle of the salt is No characteristic Absence of calcium,
made into a paste flame strontium and barium
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire

II.Systematic Analysis of Anions

S.No. Experiment Observation Inference


1.
Brisk effervescence is
Action of Dil. HCl:
noted. A colourless
To a little of the Presence of
gas is evolved which
substance about 1 ml carbonate ion (CO32-)
turned lime water
of dil. HCl is added is identified
milky
slowly and heated

2. Action of dil. H2SO4:


Little of the
No characteristic
substance is rubbed Absence of acetate
reaction
with dil. H2SO4 in a ion(CH3COO-)
watch glass
3. Action with conc.
H2SO4: No characteristic Absence of chloride
Little of conc. reaction ion(Cl-)
H2SO4 is added to a
little of the salt taken
in a dry test tube,
warmed and then
heated strongly
4. Action with conc.
H2SO4and paper ball: No characteristic Absence of nitrate
A little of salt is reaction ion(NO3-)
strongly heated conc.
H2SO4 and to the
boiling solution a
paper ball is added
and again heated
5. Action with barium No characteristic Absence of
chloride solution: reaction sulphate(SO42-) ion
Barium chloride
solution is added to
little of salt solution
taken in a test tube

III.Confirmatory Tests for Anions

S.No. Experiment Observation Inference


1. Carbonate: A small A white precipitate is Presence of
quantity of BaCl2 obtained which carbonate is
solution is added to a dissolved in dil. HCl confirmed
small amount of with a brisk
aqueous solution of effervescence of
salt taken in a test colourless gas which
tube turned lime water
milky

IV.Systematic Analysis of Cations

S.No. Experiment Observation Inference


1. Dil. HCl is added to a No characteristic
portion of aqueous reaction Absence of group I
salt solution cation ( lead ion,Pb2+)
2. Hydrogen sulphide is No characteristic Absence of group II
passed through a reaction cation (copper
portion of stock ion,Cu2+)
solution to which dil.
HCl has been added
3. To a little salt solution No characteristic Absence of group III
added excess of reaction cation (aluminium
ammonium chloride ion,Al3+)
ammonium hydroxide
drops to excess
4. Hydrogen sulphide is No characteristic Absence of group IV
passed through a reaction cation ( zinc ion, Zn2+)
portion of the salt
solution to which
NH4Cl and excess of
NH4OH have been
added
5. To a little of the salt No characteristic Absence of group V
solution added reaction cation [barium (Ba2+),
ammonium chloride, calcium (Ca2+or
ammonium hydroxide strontium (Sr2+)]
and excess of
ammonium carbonate
6. Ammonium chloride, No characteristic Absence of group VI
ammonium hydroxide reaction cation (magnesium
and sodium hydrogen ion , Mg 2+)
phosphate solutions
are added to a little of
the salt solution and
scratched the inner
side of the test tube
with a glass rod
7. Action with sodium Salt is soluble in Presence of
carbonate solution: water and no ammonium ion
A small amount of precipitate is formed (NH4+) is identified
sodium carbonate on adding Na2CO3
solution is added to a solution
little of aqueous salt
solution
8. To a little of aqueous A colourless, pungent Presence of
salt solution added a smelling gas is ammonium ion
small amount of evolved. The gas (NH4+) is confirmed.
NaOH solution and gave dense white
boiled fumes when a glass
rod dipped in Conc.
HCl is introduced
9. To about 2ml of A brown precipitate is Presence of
Nessler’s reagent obtained ammonium ion
added to the above (NH4+) is confirmed
salt solution

V.RESULT:

THE GIVEN SALT IS AMMONIUM CARBONATE [(NH4)2CO3]


SALT ANALYSIS -4
I. Preliminary Examination

S.No. Experiment Observation Inference


1. Colour and Colourless Absence of Copper,
appearance of the Iron, Cobalt,
substance are noted Manganese Nickel
salts

2. Action of heat:
A little of the salt is No characteristic Absence of carbonate
strongly heated in a reaction and acetate
clean dry test tube
3. Flame test:
Alittle of the salt is Brick red colour Presence of calcium
made into a paste ion
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire

II.Systematic Analysis of Anions

S.No. Experiment Observation Inference


1. Action of Dil. HCl:
To a little of the
No characteristic Absence of carbonate
substance about 1 ml
reaction ion (CO32-)
of dil. HCl is added
slowly and heated
2. Action of dil. H2SO4:
Little of the
No characteristic
substance is rubbed Absence of acetate
reaction
with dil. H2SO4 in a ion(CH3COO-)
watch glass
3. Action with conc. A colourless fuming
H2SO4: gas is evolved which Presence of chloride
Little of conc. gave dense white ion(Cl-) is identified
H2SO4 is added to a fumes when a glass
little of the salt taken rod dipped in
in a dry test tube, Ammonium hydroxide
warmed and then is introduced in the
heated strongly test tube

4. Action with conc.


H2SO4and paper ball: No characteristic Absence of nitrate
A little of salt is reaction ion(NO3-)
strongly heated conc.
H2SO4 and to the
boiling solution a
paper ball is added
and again heated
5. Action with barium No characteristic Absence of
chloride solution: reaction sulphate(SO42-) ion
Barium chloride
solution is added to
little of salt solution
taken in a test tube

III.Confirmatory Tests for Anions

S.No. Experiment Observation Inference


1. Chloride: To a little of A white curdy Presence of chloride
the aqueous salt precipitate is formed ion(Cl-) is confirmed
solution a few drops which dissolved in
of dil. HNO3 and excess of NH4OH
silver nitrate solution solution

IV.Systematic Analysis of Cations

S.No. Experiment Observation Inference


1. Dil. HCl is added to a No characteristic
portion of aqueous reaction Absence of group I
salt solution cation ( lead ion,Pb2+)
2. Hydrogen sulphide is No characteristic Absence of group II
passed through a reaction cation (copper
portion of stock ion,Cu2+)
solution to which dil.
HCl has been added
3. To a little salt solution No characteristic Absence of group III
added excess of reaction cation (aluminium
ammonium chloride ion,Al3+)
ammonium hydroxide
drops to excess
4. Hydrogen sulphide is No characteristic Absence of group IV
passed through a reaction cation ( zinc ion, Zn2+)
portion of the salt
solution to which
NH4Cl and excess of
NH4OH have been
added
5. To a little of the salt A white precipitate is Presence of group V
solution added obtained cation [barium (Ba2+),
ammonium chloride, calcium (Ca2+or
ammonium hydroxide strontium (Sr2+)] is
and excess of identified
ammonium carbonate
6. To a little of the salt No characteristic Absence of
solution added little precipitate. barium(Ba2+) ion
acetic acid and
potassium chromate
solution
7. A little of the salt No characteristic Absence of
solution is boiled with precipitate strontium(Sr2+) ion
acetic acid and
ammonium sulphate
is added
8. To a little of the salt White crystalline Presence of calcium
solution added precipitate insoluble ion (Ca2+) is
ammonium chloride, in acetic acid is identified
ammonium hydroxide formed
and ammonium
oxalate solutions are
added
9. Alittle of the salt is Brick red colour for Presence of calcium
made into a paste the flame is observed ion (Ca2+) is
with few drops of confirmed
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire

RESULT:

THE GIVEN SALT IS CALCIUM CHLORIDE [CaCl2]


SALT ANALYSIS -5

I. Preliminary Examination

S.No. Experiment Observation Inference


1. Colour and Colourless Absence of Copper,
appearance of the Iron, Cobalt,
substance are noted Manganese Nickel
salts

2. Action of heat:
A little of the salt is Pleasant smelling Presence of acetate
strongly heated in a inflammable vapours
clean dry test tube are evolved.
3. Flame test:
Alittle of the salt is No characteristic Absence of calcium,
made into a paste flame strontium and barium
with few drops of
conc. HCl. The paste
is brought close to a
non-luminous flame
by means of a
platinum wire

II.Systematic Analysis of Anions

S.No. Experiment Observation Inference


1. Action of Dil. HCl:
To a little of the
No characteristic Absence of carbonate
substance about 1 ml
reaction ion (CO32-)
of dil. HCl is added
slowly and heated
2. Action of dil. H2SO4:
Little of the
Vinegar like smell is Presence of acetate
substance is rubbed
observed ion(CH3COO-) is
with dil. H2SO4 in a
identified
watch glass
3. Action with conc.
H2SO4: No characteristic Absence of chloride
Little of conc. reaction ion(Cl-)
H2SO4 is added to a
little of the salt taken
in a dry test tube,
warmed and then
heated strongly

4. Action with conc.


H2SO4and paper ball: No characteristic Absence of nitrate
A little of salt is reaction ion(NO3-)
strongly heated conc.
H2SO4 and to the
boiling solution a
paper ball is added
and again heated
5. Action with barium No characteristic Absence of
chloride solution: reaction sulphate(SO42-) ion
Barium chloride
solution is added to
little of salt solution
taken in a test tube

III.Confirmatory Tests for Anions


S.No. Experiment Observation Inference
1. Acetate: To a little of A deep red Presence of acetate
aqueous solution of colouration is ion(CH3COO-) is
salt little neutral FeCl3 obtained confirmed
solution is added

IV.Systematic Analysis of Cations

S.No. Experiment Observation Inference


1. Dil. HCl is added to a No characteristic
portion of aqueous reaction Absence of group I
salt solution cation ( lead ion,Pb2+)
2. Hydrogen sulphide is No characteristic Absence of group II
passed through a reaction cation (copper
portion of stock ion,Cu2+)
solution to which dil.
HCl has been added
3. To a little salt solution No characteristic Absence of group III
added excess of reaction cation (aluminium
ammonium chloride ion,Al3+)
ammonium hydroxide
drops to excess
4. Hydrogen sulphide is No characteristic Absence of group IV
passed through a reaction cation ( zinc ion, Zn2+)
portion of the salt
solution to which
NH4Cl and excess of
NH4OH have been
added
5. To a little of the salt No characteristic Absence of group V
solution added reaction cation [barium (Ba2+),
ammonium chloride, calcium (Ca2+or
ammonium hydroxide strontium (Sr2+)]
and excess of
ammonium carbonate
6. Ammonium chloride, No characteristic Absence of group VI
ammonium hydroxide reaction cation (magnesium
and sodium hydrogen ion , Mg 2+)
phosphate solutions
are added to a little of
the salt solution and
scratched the inner
side of the test tube
with a glass rod
7. Action with sodium Salt is soluble in Presence of
carbonate solution: water and no ammonium ion
A small amount of precipitate is formed (NH4+) is identified
sodium carbonate on adding Na2CO3
solution is added to a solution
little of aqueous salt
solution
8. To a little of aqueous A colourless, pungent Presence of
salt solution added a smelling gas is ammonium ion
small amount of evolved. The gas (NH4+) is confirmed.
NaOH solution and gave dense white
boiled fumes when a glass
rod dipped in Conc.
HCl is introduced
9. To about 2ml of A brown precipitate is Presence of
Nessler’s reagent obtained ammonium ion
added to the above (NH4+) is confirmed
salt solution

RESULT:

THE GIVEN SALT IS AMMONIUM ACETATE [CH3COONH4]


ORGANIC
ANALYSIS
ORGANIC ANALYSIS -1
Aim:

Identify the functional group present in the given organic


compound.

Experiment Observations Inference


1 Dissolve a small amount brown colour of Absence of
of the organic compound bromine not unsaturation
in CCl4, then add bromine discharged
water drop wise

2 Toa little of organic A brisk Presence of


compound in a test tube, effervescence carboxylic
add a pinch of NaHCO3. group

3 Take 1 ml of neutral ferric No characteristic Absence of


chloride solution in a observation phenolic group
clean test tube and add
2-3 drops of the organic
compound.

4 To a little of the given No characteristic Absence of


organic compound add observation alcoholic group
anhydrous calcium
sulphate and shake well
to remove water. Filter
the liquid and add a small
piece of sodium metal.

5 2,4-dinitro phenyl No characteristic Absence of


hydrazine test observation carbonyl group
Take a small amount of
organic compound in a
clean test tube add
rectified spirit until the
compound just dissolves.
Now add a few drops of
2,4-dinirtophenyl
hydrazine solution. Shake
the mixture and allow to
stand 5 minutes.
6 Take about 0.2 g of solid No characteristic Absence of
potassium hydroxide in a observation amino group
test tube and add 2 ml of
ethanol. Warm the test
tube until the pallets
dissolve. To this add a
few drops of
chloroform,small amount
of the given compound
and warm gently.

Confirmatory test for


carboxylic acid

1 Litmus test
Place a drop of the given Colour changes Presence of
compound on a moist to red carboxylic
blue litmus paper group is
confirmed
2 Ester test
Take about 0.1 g of the Fruity smell Presence of
organic compound ,1 ml carboxylic
of ethyl alcohol and 1-2 group is
drops of conc.H2SO4 in a confirmed
test tube. Heat the
reaction mixture on a
water bath for five
minutes. Pour the
reaction mixture in a
beaker containing water.

Result :

The given organic compound contains –COOH s the functional


group
ORGANIC ANALYSIS -2

Aim:

Identify the functional group present in the given organic


compound.
Experiment Observations Inference
1 Dissolve a small amount brown colour of Absence of
of the organic compound bromine not unsaturation
in CCl4, then add bromine discharged
water drop wise.

2 Toa little of organic No characteristic Absence of


compound in a test tube, observation carboxylic
add a pinch of NaHCO3. group

3 Take 1 ml of neutral ferric Violet Presence of


chloride solution in a colouration phenol
clean test tube and add 2-
3 drops of the organic
compound.

4 To a little of the given No characteristic Absence of


organic compound add observation alcoholic group
anhydrous calcium
sulphate and shake well
to remove water. Filter the
liquid and add a small
piece of sodium metal.

5 2,4-dinitro phenyl No characteristic Absence of


hydrazine test observation carbonyl group
Take a small amount of
organic compound in a
clean test tube add
rectified spirit until the
compound just dissolves.
Now add a few drops of
2,4-dinirtophenyl
hydrazine solution. Shake
the mixture and allow to
stand 5 minutes.
6 Take about 0.2 g of solid No characteristic Absence of
potassium hydroxide in a observation amino group
test tube and add 2 ml of
ethanol. Warm the test
tube until the pallets
dissolve. To this add a
few drops of
chloroform,small amount
of the given compound
and warm gently.

Confirmatory test for


phenol

1 Litmus test
Place a drop of the given Colour changes Presence of
compound on a moist to red phenol is
blue litmus paper confirmed

2 Liebermann’s test
Place sodium nitrite in a A deep blue or
clean dry test tube and green Presence of
add the given organic colouration phenol is
compound in it. Heat develops confirmed
gently for half a minute
and allow it to cool. Then
add conc. H2SO4 and
shake the tube.

Result :

The given organic compound contains Phenol as the functional


group.
ORGANIC ANALYSIS -3
Aim:

Identify the functional group present in the given organic


compound.
Experiment Observations Inference
1 Dissolve a small amount brown colour of Absence of
of the organic compound bromine not unsaturation
in CCl4, then add bromine discharged
water drop wise
2 Toa little of organic No characteristic Absence of
compound in a test tube, observation carboxylic
add a pinch of NaHCO3. group

3 Take 1 ml of neutral ferric No characteristic


chloride solution in a observation Absence of
clean test tube and add 2- phenolic group
3 drops of the organic
compound.
4 To a little of the given No characteristic
organic compound add observation Absence of
anhydrous calcium alcoholic group
sulphate and shake well
to remove water. Filter the
liquid and add a small
piece of sodium metal.
5 2,4-dinitro phenyl Formation of
hydrazine test yellow or orange Presence of
Take a small amount of crystals carbonyl group
organic compound in a
clean test tube add
rectified spirit until the
compound just dissolves.
Now add a few drops of
2,4-dinirtophenyl
hydrazine solution. Shake
the mixture and allow to
stand 5 minutes.

6 Dissolve 0.5 ml of the Appearance of Presence of


given organic compound pink colour aldehydic group
in alcohol and add Schiff’s
reagent. Shake well
7 Take about 0.2 g of solid
potassium hydroxide in a No characteristic Absence of
test tube and add 2 ml of observation amino group
ethanol. Warm the test
tube until the pallets
dissolve. To this add a
few drops of
chloroform,small amount
of the given compound
and warm gently.

Confirmatory test for


aldehydes
1 Tollen’s test
Place 1ml of silver nitrate A shining mirror Presence of
solution in a clean dry test is formed. aldehydic group
tube and add 2-3 ml of is confirmed.
dil.NaOH solution . A
brown ppt. forms. Now
add dilute ammonia
solution drop wise until
the brown ppt. of silver
oxide just dissolves. To
this add a little of the
given organic compound
and warm the test tube on
a water bath for 5
minutes.

2 Fehling’s test Appearance of a Presence of


Take an equal amount of red ppt. aldehydic group
Fehling’s solutions A and is confirmed.
B in a test tube. Add 4-5
drops of the given organic
compound and warm the
test tube in a hot water
bath for 5 minutes.

Result :

The given organic compound contains Aldehyde(-CHO) as the


functional group.
ORGANIC ANALYSIS -4
Aim:

Identify the functional group present in the given organic


compound.
Experiment Observations Inference
1 Dissolve a small amount brown colour of Absence of
of the organic compound bromine not unsaturation
in CCl4, then add bromine discharged
water drop wise

2 Toa little of organic No characteristic Absence of


compound in a test tube, observation carboxylic
add a pinch of NaHCO3. group

3 Take 1 ml of neutral ferric No characteristic Absence of


chloride solution in a observation phenolic group
clean test tube and add 2-
3 drops of the organic
compound.

4 To a little of the given No characteristic Absence of


organic compound add observation alcoholic group
anhydrous calcium
sulphate and shake well
to remove water. Filter the
liquid and add a small
piece of sodium metal.

5 2,4-dinitro phenyl Formation of Presence of


hydrazine test yellow or orange carbonyl group
Take a small amount of crystals
organic compound in a
clean test tube add
rectified spirit until the
compound just dissolves.
Now add a few drops of
2,4-dinirtophenyl
hydrazine solution. Shake
the mixture and allow to
stand 5 minutes.
6 Dissolve 0.5 ml of the No characteristic Presence of
given organic compound observation ketone
in alcohol and add Schiff’s
reagent. Shake well

7 Take about 0.2 g of solid No characteristic Absence of


potassium hydroxide in a observation amino group
test tube and add 2 ml of
ethanol. Warm the test
tube until the pallets
dissolve. To this add a
few drops of
chloroform,small amount
of the given compound
and warm gently.

Confirmatory test for


ketones

1 Sodium bisulphite test Formation of Presence of


Take 2 ml of a saturated crystalline white carbonyl group
solution of sodium ppt.
bisulphite in a test tube
and add 1 ml of the given
compound

2 Sodium nitroprusside test A red Presence of


Dissolve a crystal of colourarion ketonic group
sodium nitroprusside in 1
ml of distilled water and
then add a little of the
given organic compound.
Shake well and NaOH
solution drop wise.

RESULT:

The given organic compound contains ketone( -CO-) as the


functional group.
ORGANIC ANALYSIS -5

Aim:
To identify which of the following A and B contain starch and
glucose
Experiment Observation Inference
1 Fehling’s test
Toa little of the given A: Red A may be
samples add Fehling’s precipitate glucose
solution A and B.Heat it
on a water bath B: no B may be
characteristic starch
change

2 Benedict test
To a little of the given
solutions add Benedict A:reddish ppt. A contains
reagent. Keep the test glucose
tubes in a boiling water B: no
bath. characteristic B contains
change starch

3 Iodine test
To the aqueous A: no
suspension of the characteristic A contains
sample,add 1-2 drops of change glucose
iodine solution
B: appearance of
blue colouration B contains
starch

Result :

Sample A contains glucose and sample B contains starch


ORGANIC ANALYSIS -6
Aim:

Identification of proteins from the given samples A and B


Experiment Observation Inference
1 BiuretTest

Add a small amount of A: bluish violet A: protein is


NaOH solution and 4-5 colouration present
drops of 1% CuSO4 B: no B:protein is
solution to both the characteristic absent
samples change

2 Xanthoproteic test A: yellow ppt. A: protein is


To a little of the given B: : no present
samples add con.HNO3 characteristic B:protein is
change absent
3 Ninhydrin test
To a little of the given A: intense blue A: protein is
solutions add Ninhydrin colouration present
solutions B: : no B:protein is
characteristic absent
change

RESULT:
Sample A contains protein

You might also like