Experiment -3

Volumetric Analysis - NaOH x Oxalic acid

[To be written on RHS of the record]

AIM:
To determine the strength and molarity of given sodium hydroxide solution using a
standard solution of M/20 Oxalic acid.
THEORY:

Indicator: Phenolphthalein
End point: Colourless to pale pink
Reaction type: Neutralisation reaction
Pipette solution: 10 mL M/20 Oxalic acid
Burette solution: NaOH

PROCEDURE:
Weigh 0.63g Oxalic acid and transfer into a 100mL standard flask through a funnel
and make upto the mark by adding distilled water. Pipette out 10mL into the titration
flask and add 1-2 drops of Phenolphthalein indicator and titrate against NaOH solution
in the burette, until a permanent pale pink colour is obtained. Repeat the experiment
until concordant readings are obtained.
[To be written on LHS of the record]
OBSERVATIONS AND CALCULATIONS:
Molarity of oxalic acid solution (M1) = 0.05M
Volume of oxalic acid solution (V1) = 10mL
M1V1 = 1
M2V2 2
Sl No Burette readings Vol of NaOH used (mL)
Initial (mL) Final (mL)
1
2
3
Concordent readings = ………mL

M/20 oxalic acid calculation:

Ti find Molarity of NaOH:

MNaOH = ……..mol/L
Strength of NaOH solution = MNaOH x molar mass = MNaOH x 40 = g/L

RESULT:
Molarity of NaOH solution = ……….M
Strength of NaOH solution = ……….g/L
 Experiment -4
Volumetric Analysis – Na2CO3 x HCl

[To be written on RHS of the record]

AIM:
To determine the strength and molarity of given hydrochloric acid solution using a
standard solution of M/20 sodium carbonate.
THEORY:

Indicator: Methyl orange

End point: Orange to pink
Reaction type: Neutralisation reaction
Pipette solution: 10 mL M/20 sodium carbonate
Burette solution: HCl solution

PROCEDURE:
Weigh 0.53g sodium carbonate and transfer into a 100mL standard flask through a
funnel and make upto the mark by adding distilled water. Pipette out 10mL into the
titration flask and add 1-2 drops of Methyl orange indicator and titrate against HCl
solution in the burette, until a colour change of orange to pink is obtained. Repeat the
experiment until concordant readings are obtained.

[To be written on LHS of the record]

OBSERVATIONS AND CALCULATIONS:

Molarity of sodium carbonate solution (M1) = 0.05M
Volume of sodium carbonate (V1) = 10mL
M1V1 = 1
M2V2 2
Sl No Burette readings Vol of HCl used (mL)
Initial (mL) Final (mL)
1
2
3
Concordent readings = ………mL

M/20 sodium carbonate calculation

To find Molarity of HCl:

MHCl = ……..mol/L
Strength of HCl solution = MHCl x molar mass = MHCl x 36.5 = g/L

RESULT:
Molarity of HCl solution = ……….M
Strength of HCl solution = ……….g/L
 SALT ANALYSIS : (Magnesium Sulphate)
AIM:
To identify the cation and anion in the given inorganic salt.
PHYSICAL EXAMINATION OF THE SALT:
Sl No Experiment Observation Inference
1 Colour of the salt is noted Colourless Absence of Co3+, Fe2+, Fe3+,
Ni2+ etc
2 Odour of the salt is noted No characteristic smell Absence of NH4+ and
CH3COO-
3 Deliquescence Not deliquescent Absence of chlorides &
nitrates of Zn2+ or Mg2+

PRELIMINARY EXPERIMENTS
Sl No Experiment Observation Inference
1 Dry heating test: No characteristic change Absence of NH4+, NO3-,
A pinch of the salt is Al3+ , CH3COO- etc
heated in a dry test tube

TESTS FOR ANIONS:

Sl No Experiment Observation Inference
1 Dil.H2SO4 test: No characteristic change Absence of CO32-
To the salt add dil. H2SO4
in a test tube.

2 Conc.H2SO4 test: No characteristic fumes Absence of Cl- and Br –

To the salt add Conc.
H2SO4 in a test tube.

Add copper turnings and

heated. No characteristic fumes Absence of NO3-
3 Test for oxalate: No characteristic change Absence of C2O42-
To the salt add conc.
H2SO4 and KMnO4
4 Test for acetate: No characteristic change Absence of CH3COO-
To the salt add oxalic acid
and water
5 BaCl2 test: White precipitate Presence of SO42-
To the salt add barium
chloride solution.

TESTS FOR CATIONS:

Sl No Experiment Observation Inference
1 Group 0 test: No characteristic change Absence of Group 0 (NH4+)
 To the salt add
NaOH and heated
2 Group 1 test: No characteristic change Absence of Group 1 (Pb2+)
To the salt add dil.
HCl
3 Group II test: No characteristic change Absence of Group II (Pb2+)
To the salt add dil.
HCl and H2S
4 Group III test: No characteristic change Absence of Group III (Al3+)
To the salt add solid
NH4Cl and NH4OH
5 Group IV test: No characteristic change Absence of Group IV (Zn2+)
To the salt add solid
NH4Cl and NH4OH
and H2S
6 Group V test: No characteristic change Absence of Group V (Ca2+,
To the salt add solid Ba2+, Sr2+)
NH4Cl and NH4OH
and (NH4)2CO3
7 Group VI test: White precipitate Presence of Group VI
To the salt add solid (Mg2+)
NH4Cl and NH4OH
and ammonium
phosphate

CONFIRMATORY TEST FOR ANION:

Sl NoExperiment Observation Inference
1 Lead acetate test: White precipitate SO42- is confirmed.
To the salt add lead
acetate solution
CONFIRMATORY TEST FOR CATION:
Sl No Experiment Observation Inference
1 Magneson reagent Blue precipitate Mg2+ is confirmed.
test:
To the O.S add
Magneson reagent
2 Cobalt nitrate test: Pink/ white tinted ash Mg2+ is confirmed.
Salt is mixed with
conc.HNO3 and
cobalt nitrate. A
filter paper is dipped
into it and burnt into
ash.

RESULT:
The given inorganic salt contains Mg2+ as cation and SO42- as anion.
(EQUATIONS TO BE WRITTEN ON LHS)

1. Barium chloride test

s
2. Lead acetate test

3. Ammonium phosphate test

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

 SALT ANALYSIS : (Strontium Chloride)
AIM:
To identify the cation and anion in the given inorganic salt.
PHYSICAL EXAMINATION OF THE SALT:
Sl No Experiment Observation Inference
1 Colour of the salt is noted Colourless Absence of Co3+, Fe2+, Fe3+,
Ni2+ etc
2 Odour of the salt is noted No characteristic smell Absence of NH4+ and
CH3COO-
3 Deliquescence Not deliquescent Absence of chlorides and
nitrates of Zn2+ or Mg2+

PRELIMINARY EXPERIMENTS
Sl No Experiment Observation Inference
1 Dry heating test: No characteristic Absence of NH4+,
A pinch of the salt is observation CH3COO-, NO3- etc
heated in a dry test tube

TESTS FOR ANIONS:

Sl No Experiment Observation Inference
1 Dil.H2SO4 test: No characteristic change Absence of CO32-
To the salt add dil. H2SO4
in a test tube.

2 Conc.H2SO4 test: White fumes Presence of Cl -

To the salt add Conc. (Colourless gas giving
H2SO4 in a test tube. dense white fumes with
a glassrod of NH4OH
Add copper turnings and
heated

TESTS FOR CATIONS:

Sl No Experiment Observation Inference
1 Group 0 test: No characteristic change Absence of Group 0 (NH4+)
To the salt add
NaOH and heated
2 Group 1 test: No characteristic change Absence of Group 1 (Pb2+)
 To the salt add dil.
HCl
3 Group II test: No characteristic change Absence of Group II (Pb2+)
To the salt add dil.
HCl and H2S
4 Group III test: No characteristic change Absence of Group III (Al3+)
To the salt add solid
NH4Cl and NH4OH
5 Group IV test: No characteristic change Absence of Group IV (Zn2+)
To the salt add solid
NH4Cl and NH4OH
and H2S
6 Group V test: White precipitate Presence of Group V (Ca2+,
To the salt add solid Ba2+, Sr2+)
NH4Cl and NH4OH
and (NH4)2CO3

CONFIRMATORY TEST FOR ANION:

Sl No Experiment Observation Inference
1 AgNO3 test: White precipitate Cl- is confirmed.
To the salt add
dil.HNO3,
heated,cooled and
add AgNO3 solution

CONFIRMATORY TEST FOR CATION:

Sl No Experiment Observation Inference
1 Ammonium White precipitate Sr2+ is confirmed.
sulphate:
To the O.S add
ammonium sulphate
solution.

RESULT:
The given inorganic salt contains Sr2+ as cation and Cl - as anion.

(EQUATIONS TO BE WRITTEN ON LHS)

1. AgNO3 test
2. Ammonium sulphate test
 EXPERIMENT - 13
SALT ANALYSIS No: 3 (Aluminium Sulphate)
AIM:
To identify the cation and anion in the given inorganic salt.
PHYSICAL EXAMINATION OF THE SALT:
Sl No Experiment Observation Inference
1 Colour of the salt is noted Colourless Absence of Co3+, Fe2+, Fe3+,
Ni2+ etc
2 Odour of the salt is noted No characteristic smell Absence of NH4+ and
CH3COO-
3 Deliquescence Not deliquescent Absence of Zn2+ or Mg2+

PRELIMINARY EXPERIMENTS
Sl No Experiment Observation Inference
1 Dry heating test: Swelling May be Al3+
A pinch of the salt is
heated in a dry test tube
2 Flame test: No characteristic colour Absence of Sr2+, Ca2+,
Make a paste of salt with Ba2+, Pb2+
conc.HCl in a watch glass
and shown to flame with a
platinum loop.
3 Cobalt nitrate test: Blue ash Presence of Al3+
Salt is mixed with
conc.HNO3 and cobalt
nitrate in a watch glass, a
filter paper dipped in it is
burnt to ash.

TESTS FOR ANIONS:

Sl No Experiment Observation Inference
1 Dil.H2SO4 test: No characteristic change Absence of CO32-
To the salt add dil. H2SO4
in a test tube.

2 Conc.H2SO4 test: No characteristic fumes Absence of Cl- and Br –

To the salt add Conc.
H2SO4 in a test tube.
 Add copper turnings and No characteristic fumes Absence of NO3-
heated.
3 Test for oxalate: No characteristic change Absence of C2O42-
To the salt add conc.
H2SO4 and KMnO4
4 Test for acetate: No characteristic change Absence of CH3COO-
To the salt add oxalic acid
and water
5 BaCl2 test: White precipitate Presence of SO42-
To the salt add barium
chloride solution.
TESTS FOR CATIONS:
Sl No Experiment Observation Inference
1 Group 0 test: No characteristic change Absence of Group 0 (NH4+)
To the salt add
NaOH and heated
2 Group 1 test: No characteristic change Absence of Group 1 (Pb2+)
To the salt add dil.
HCl
3 Group II test: No characteristic change Absence of Group II (Pb2+)
To the salt add dil.
HCl and H2S
4 Group III test: White gelatinous precipitate Presence of Group III (Al3+)
To the salt add solid
NH4Cl and NH4OH

CONFIRMATORY TEST FOR ANION:

Sl No Experiment Observation Inference
1 Lead acetate test: White precipitate SO42- is confirmed.
To the salt add lead
acetate solution

CONFIRMATORY TEST FOR CATION:

Sl No Experiment Observation Inference
1 Lake test: Blue precipitate Al3+ is confirmed.
Group III ppt is
dissolved in dil HCl
and add blue litmus
solution followed by
NH4OH
RESULT:
The given inorganic salt contains Al3+ as cation and SO42- as anion.

(EQUATIONS TO BE WRITTEN ON LHS)

1. BaCl2 test

2. Lead acetate test

3. Lake test
 EXPERIMENT - 12
SALT ANALYSIS No: 2 (Lead Nitrate)
AIM:
To identify the cation and anion in the given inorganic salt.
PHYSICAL EXAMINATION OF THE SALT:
Sl No Experiment Observation Inference
1 Colour of the salt is noted Colourless Absence of Co3+, Fe2+, Fe3+,
Ni2+ etc
2 Odour of the salt is noted No characteristic smell Absence of NH4+ and
CH3COO-
3 Deliquescence Not deliquescent Absence of Zn2+ or Mg2+

PRELIMINARY EXPERIMENTS
Sl No Experiment Observation Inference
1 Dry heating test:
A pinch of the salt is Crackling sound with red May be NO3-
heated in a dry test tube fumes
2 Flame test: Dull white flame Pb2+ may be present
Make a paste of salt with
conc.HCl in a watch glass
and shown to flame with a
platinum loop.
3 Cobalt nitrate test: No characteristic colour Absence of Al3+ ,Zn2+
Salt is mixed with ,Mg2+
conc.HNO3 and cobalt
nitrate in a watch glass, a
filter paper dipped in it is
burnt to ash.

TESTS FOR ANIONS:

Sl No Experiment Observation Inference
1 Dil.H2SO4 test: No characteristic change Absence of CO32-
To the salt add dil. H2SO4
in a test tube.

2 Conc.H2SO4 test: No characteristic fumes Absence of Cl- and Br –

To the salt add Conc.
H2SO4 in a test tube.
 Add copper turnings and Brown fumes Presence of NO3-
heated.
TESTS FOR CATIONS:
Sl No Experiment Observation Inference
1 Group 0 test: No characteristic change. Absence of Group 0 (NH4+)
To the salt add
NaOH and heated
2 Group 1 test: White precipitate Presence of Group 1 (Pb2+)
To the salt add dil.
HCl
3 Group II test: Black precipitate Presence of Group II (Pb2+)
To the salt add dil.
HCl and H2S

CONFIRMATORY TEST FOR ANION:

Sl No Experiment Observation Inference
1 Brown ring test: A brown ring is formed at the NO3- is confirmed.
To the salt add junction of two layers
freshly prepared
FeSO4 solution and
add conc. H2SO4
through the sides of
test tube

CONFIRMATORY TEST FOR CATION:

Sl No Experiment Observation Inference
1 Potassium iodide Yellow precipitate Pb2+ is confirmed.
test:
To the salt add KI
solution
2 Potassium Yellow precipitate Pb2+ is confirmed.
chromate test:
To the salt add
K2CrO4 solution.

RESULT:
The given inorganic salt contains Pb2+ as cation and NO3- as anion.
(EQUATIONS TO BE WRITTEN ON LHS)
1. Brown ring test

2. KI test

3. K2CrO4 test
 EXPERIMENT - 19
SALT ANALYSIS No: 9 (Ammonium Bromide)
AIM:
To identify the cation and anion in the given inorganic salt.
PHYSICAL EXAMINATION OF THE SALT:
Sl No Experiment Observation Inference
1 Colour of the salt is noted Colourless Absence of Co3+, Fe2+, Fe3+,
Ni2+ etc
2 Odour of the salt is noted No characteristic smell Presence of NH4+
3 Deliquescence Not deliquescent Absence of Zn2+ or Mg2+

PRELIMINARY EXPERIMENTS
Sl No Experiment Observation Inference
1 Dry heating test: Sublimation Presence of NH4+
A pinch of the salt is
heated in a dry test tube

TESTS FOR ANIONS:

Sl No Experiment Observation Inference
1 Dil.H2SO4 test: No characteristic change Absence of CO32-
To the salt add dil. H2SO4
in a test tube.

2 Conc.H2SO4 test: Reddish brown fumes May be Br-

To the salt add Conc.
H2SO4 in a test tube.

TESTS FOR CATIONS:

Sl No Experiment Observation Inference
1 Group 0 test: Colourless gas giving dense Presence of Group 0 (NH4+)
To the salt add white fumes when a glass rod
NaOH and heated dipped in conc. HCl is shown
at the mouth of the test tube.
CONFIRMATORY TEST FOR ANION:
Sl No Experiment Observation Inference

Salt solution + Pale Yeloow ppt Br- confirmed

Silver nitrate solut

CONFIRMATORY TEST FOR CATION:

Sl No Experiment Observation Inference
1 Nessler’s test: Brown precipitate NH4+ is confirmed.
To the salt add
NaOH and heated
and add Nessler’s
reagent.

RESULT:
The given inorganic salt contains NH4+ as cation and Br as anion.
AIM:

To detect the presence of elements (Nitrogen, Sulphur, Chlorine, Bromine & Iodine)
in the given organic compound.

Theory:

Lassaigne’s Sodium fusion extract will be prepared using the given organic sample.

The covalently bonded atoms in the organic compound get converted to its ionic
form.

Procedure:

Preparation of sodium fusion extract (SFE):

A small amount of organic substance is fused with a small quantity of sodium metal in
a fusion tube. The red hot fusion tube is then plunged into distilled water and the
contents are boiled for few minutes, then cooled and filtered. The filtrate obtained is
called sodium fusion extract (SFE) or Lassaigne’s extract.

1. SAMPLE I:

Experiment Observation Inference

To the SFE, add 2mL Prussian blue Nitrogen is confirmed

freshly prepared FESO4, colouration
heated and add 1-2
drops of FeCl3 solution
followed by 1-2 drops of
Conc. HCl.

To the SFE, add sodium Purple colouration Sulphur is confirmed

nitroprusside solution.

To the SFE, add acetic Black precipitate Sulphur is confirmed.

acid and lead acetate
solution.

To the SFE, add equal Blood red colouration Both Nitrogen and
quantity of FeCl3 sulphur are confirmed.
solution.
To the SFE, add dil nitric White precipitate Chlorine is confirmed.
acid and AgNO3 soluble in NH4OH
solution.
Pale yellow ppt partially Bromine is confirmed.
soluble in NH4OH

Yellow ppt insoluble in Iodine is confirmed.

NH4OH

RESULT:

Sample I contains ………………………………

2. SAMPLE II:

Experiment Observation Inference

To the SFE, add 2mL Prussian blue Nitrogen is confirmed

freshly prepared FESO4, colouration
heated and add 1-2
drops of FeCl3 solution
followed by 1-2 drops of
Conc. HCl.

To the SFE, add sodium Purple colouration Sulphur is confirmed

nitroprusside solution.

To the SFE, add acetic Black precipitate Sulphur is confirmed.

acid and lead acetate
solution.

To the SFE, add equal Blood red colouration Both Nitrogen and
quantity of FeCl3 sulphur are confirmed.
solution.

To the SFE, add dil nitric White precipitate Chlorine is confirmed.

acid and AgNO3 soluble in NH4OH
solution.
Pale yellow ppt partially Bromine is confirmed.
soluble in NH4OH

Yellow ppt insoluble in Iodine is confirmed.

NH4OH

RESULT:

Sample II contains ………………………………

CHEMICAL EQUATIONS INVOLVED:

For Nitrogen:

For Sulphur:

For Nitrogen & Sulphur:

For halogens: