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Procedure :
Dissolve 5ml of aniline in 20 ml 0f dil.HCl in a boiling tube and cool in an ice bath.
Dissolve 8 g NaNO2 in 10 15 ml of distilled water in a boiling tube and cool in ice bath.
Add cooled aq. solution of NaNO2 slowly to cooled solution of aniline. Shake after each
addition.
Add few pieces of ice to reaction mixture. If diazotization is complete, the solution changes
starch iodide paper to blue.
Dissolve 3 g of NaOH in 10 ml of water in another boiling tube. Add 8 ml of 2- Naphthol to it
slowly with shaking. Cool in an ice bath.
Add solution of benzene diazonium chloride to the solution of 2- Naphthol in NaOH in small
quantities with shaking.
Orange dye is formed. Filter it in a buchner funnel. Wash the dye with water and dry it
between folds of filter paper. Weigh it.
Result :
Yield of crystals 7 g
Colour of crystals Orange
Precautions
Reaction mixture should be properly cooled.
pH of coupling reaction should be between 9 -10.
Observation
Inference
Fehlings Test
Sample + Fehlings solution + Yellow or red precipitate
warm in water bath.
Benedicts Test
Sample + Benedicts solution + Red precipitate
warm in water bath.
Conc. H2SO4 Test
Sample + Conc. H2SO4
Carbohydrate present
Carbohydrate present
Carbohydrate present
Observation
Inference
Sample dissolves
Experiment 3
Aim : To detect the presence of protein in the given foodstuff.
Experiment
xanthproteic Test
Sample + few ml of conc. HNO3
Shake and leave undisturbed.
Millons Test
Sample + few drops of mercuric nitrate+
1 drop dil. HCl + Boil , Cool + 1drop NaNO3
+ Heat mixture
Biuret Test
Sample + 10% NaOH + dil. CuSO4
Ninhydrin Test
Sample + 0.1% ninhydrin solution + boil for 1
minute
Observation
Inference
Proteins
present
Proteins
present
Violet colour
Proteins
present
Proteins
present
Observation
Inference
Presence of unsaturation
Presence of unsaturation
Experiment 2
Aim : To test for the presence of alcoholic group in a given organic sample.
Experiment
Ester Test
Sample + few drops of acetic acid +
Conc. H2SO4
Warm in a water bath.
Sample + small piece of Na metal
Iodoform Test
Sample + NaOH solution + solid I2
+ warm
Observation
Inference
Pleasant smell
Ester present
Yellow precipitate
Experiment 3
Aim : To test for the presence of phenolic group in organic sample
Experiment
Litmus Test
Sample + blue litmus
FeCl3 Test
Sample + small amount of FeCl3
Observation
Inference
Presence of phenolic
group
Presence of phenolic
group
White precipitate
Presence of phenolic
group
Green or brown
precipitate
Presence of phenolic
group
.
Experiment 4
Aim : To test for the presence of aldehyde group in organic sample.
Experiment
2,4 Dinitrophenyl hydrazine
Test
2,4 DNP + sample
Schiffs Test
Sample + Schiffs Reagent
Fehlings Test
Sample + Fehlings solution +
warm in water bath
Tollens Test
Sample + Tollens solution +
warm in water bath
Observation
Inference
Presence of aldehyde
group
Pink colour
Presence of aldehyde
group
Presence of aldehyde
group
Presence of aldehyde
group
Experiment 5
Aim : To test for the presence of carboxylic acid group in organic sample.
Experiment
Litmus Test
Sample + blue litmus
Observation
Inference
Presence of carboxylic
acid group
Presence of carboxylic
acid group
NaOH Test
Sample + NaOH solution
Sample is soluble
Presence of carboxylic
acid group
FeCl3 Test
Sample + water + NH4OH . Boil to remove
NH3. Cool and add neutral FeCl3
Red or Yellow
precipitate
Presence of carboxylic
acid group
Aim : To determine the molarity of KMnO4 by titrating it against standard solution of oxalic
acid.
Theory : Potassium permanganate oxidizes oxalic acid into carbon dioxide in acidic medium at a
temperature around 60C and itself gets reduced to colourless ions.
2 KMnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5[O]
COOH
60C
|
+ [O] 2CO2 + H2O ] x 5
COOH
2 KMnO4 + 3H2SO4 + 5(COOH)2 K2SO4 + 2MnSO4 + 10CO2 + 10 H2O
Preparation of standard Solution :
250 ml of M/20 oxalic acid requires = 1.575 g of oxalic acid.
Indicator : KMnO4 is self indicator
End point : Colourless to pink
Procedure :
Rinse and fill burette with given KMnO4 solution.
Rinse the pipette with M/20 oxalic acid and pipette out 10.0 ml of it in a washed titration
flask.
Add half test tube of dilute H2SO4 to flask, shake and heat it to around 60C
Note initial reading of burette ( upper meniscus)
Now add KMnO4 from burette till a permanent light pink colour is imparted to solution in
titration flask.
Note the final reading in the Burette.
Repeat 4 - 5 times to get 3 concordant readings.
Result : The molarity of KMnO4 solution is ..M
Record of Readings
Molarity of oxalic acid = M/20
Volume of oxalic acid = 10 ml
S No.
Burette Reading
Initial
1.
2.
Final
Volume of
KMnO4 used (ml)
Calculations
KMnO4
=
Oxalic acid
a1 x V1 x M1 = a2 x V2 x M2
a2 x V2 x M2
M1 =
=
a1 x V1
2 x 10 x M/20
5 X V1
= 1/(5V1) M
= M
Record of Readings
Molarity of Mohrs salt = M/20
Volume of Mohrs salt = 10 ml
S No.
Burette Reading
Initial
Volume of
KMnO4 used (ml)
Final
1.
2.
Calculations
(i) KMnO4
=
Mohrs salt
a1 x V1 x M1 = a2 x V2 x M2
a2 x V2 x M2
M1 =
=
a1 x V1
2 x 20 x M/20
10 X V1
= 2/(10V1) M
= M
(ii) Strength of KMnO4 solution = molarity x molecular mass
= 2/(10V1) M x 158
= .g/l.
Salt Analysis
1. Aim:
Experiment
Nature of the salt
Original solution
+
NaOH + heat
Original solution
+
Nesslers reagent
Observation
White crystalline, dissolves
in water.
Gas with pungent smell of ammonia
evolved.
Forms dense white fumes with HCl
Inference
Brown precipitate
NH4+
confirmed
Experiment
Preliminary Test
Confirmatory Test
Water extract + silver nitrate
solution
Observation
No characteristic change
Colourless gas with pungent
smell evolved
Dense white fumes are
formed.
the presence
NH4+ indicated
cation in the
sample.
Inference
Absence of
CO32-, S2-, SO32-, NO2indicated
Cl- indicated
Cl- confirmed
2. Aim: To analyse the presence of anion and cation in the given salt sample.
Observation
of anion and
given salt
Experiment
To analyse
Inference
Preliminary Test
No characteristic change
Confirmatory Test
Water extract + ferrous
sulphate + conc. H2SO4
along sides of test tube
Experiment
Nature of the salt
Original solution +
Absence of
CO32-, S2-, SO32-, NO2indicated
NO3- indicated
NO3- confirmed
Observation
White crystalline, dissolves
in water.
Inference
No characteristic change
NaOH + heat
Result:
The
given salt
is
Pb(NO3)2
3. Aim: To analyse the presence of anion and cation in the given salt sample.
Experiment
Preliminary Test
Observation
No characteristic change
Inference
Absence of
CO32-, S2-, SO32-, NO2indicated
No characteristic change
Salt + conc. H2SO4
White precipitate insoluble
Absence of
Cl-, Br-, I-, NO3-, CH3COO-,
C2O4-
Confirmatory Test
Water extract + lead
acetate
in dilute HCl.
Indicated
SO42- indicated
SO42- confirmed
Experiment
Nature of the salt
Original solution +
Observation
White crystalline, dissolves
in water.
Inference
No characteristic change
Absence of NH4+
NaOH + heat
indicated
No characteristic change
Absence of Group I
indicated
No characteristic change
Absence of Group II
indicated
Al3+ indicated
Into 2 parts
Part 1 + NaOH
Part 2 + blue litmus+ NH4OH
dropwise
Al3+ confirmed
Al3+ confirmed
Experiment
Nature of the salt
Original solution +
Observation
White crystalline, dissolves
in water.
Inference
No characteristic change
No characteristic change
Absence of Group I
NaOH + heat
Original solution +
Dilute HCl
Original solution +
Dilute HCl + H2S gas
indicated
No characteristic change
Absence of Group II
indicated
No characteristic change
Part 1 + NaOH
Part 2 + K4[Fe(CN)6]
Experiment
Preliminary Test
White precipitate
Dissolve precipitate in HCl.
Boil off H2S. Divide into 2
parts
White precipitate soluble in
excess NaOH.
White or bluish white
precipitate.
Observation
No characteristic change
Zn2+ indicated
Zn2+ confirmed
Zn2+ confirmed
Inference
Absence of
CO32-, S2-, SO32-, NO2indicated
No characteristic change
Salt + conc. H2SO4
Salt + BaCl2 solution
Confirmatory Test
Water extract + lead
acetate
Absence of
Cl-, Br-, I-, NO3-, CH3COO-,
C2O4Indicated
SO42- indicated
SO42- confirmed
Experiment
Nature of the salt
Original solution +
Observation
White crystalline, dissolves
in water.
Inference
No characteristic change
NaOH + heat
Absence of Group I
Original solution +
Dilute HCl
Original solution +
Dilute HCl + H2S gas
Original solution + NH4Cl(s) +
NH4OH
No characteristic change
indicated
Absence of Group II
No characteristic change
indicated
Absence of Group III
No characteristic change
indicated
Absence of Group IV
Group V indicated
White precipitate
Dissolve precipitate in acetic
acid and divide into 3 parts
Yellow precipitate
+ NH4OH + (NH4)2CO3
Experiment
Preliminary Test
indicated
No characteristic change
Observation
No characteristic change
Inference
Absence of
CO32-, S2-, SO32-, NO2indicated
Cl- confirmed
Confirmatory Test
Water extract + silver nitrate
solution
Ba2+ confirmed
6. Aim: To analyse the presence of anion and cation in the given salt sample.
Observation
Inference
No characteristic change
Absence of
CO32-, S2-, SO32-, NO2indicated
Experiment
Preliminary Test
No characteristic change
Salt + conc. H2SO4
Absence of
No characteristic change
Salt + BaCl2 solution
Salt + conc. HNO3 + heat
+ ammonium molybdate
Experiment
Nature of the salt
Original solution +
Observation
White crystalline, dissolves
in water.
Inference
No characteristic change
NaOH + heat
Absence of Group I
Original solution +
Dilute HCl
Original solution +
Dilute HCl + H2S gas
No characteristic change
Absence of Group II
No characteristic change
indicated
Absence of Group III
No characteristic change
indicated
Absence of Group IV
No characteristic change
indicated
No characteristic change
indicated
Absence of Group V
indicated
White precipitate on
scratching
Inner side of test tube
Mg2+ confirmed