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Preparation of Iodoform

Aim : To prepare a pure sample of iodoform.


Chemicals :
Acetone 5 ml
Iodine 5 g
NaOH 5 %
Methylated spirit
Theory :
CH3COCH3 + 4I2 + 4NaOH CHI3 + 3NaI + CH3COONa + 2H2O
Procedure:
Dissolve 5 g of iodine in 5 ml acetone in a conical flask.
Add 5 % sodium hydroxide solution slowly with shaking until the colour of iodine is
discharged.
Allow contents of flask to stand for 10 15 minutes.
Filter the yellow precipitate of iodoform through Buchner funnel
Wash the precipitate with cold water.
Dry precipitate between filter paper and weigh it.
Result :
Yield of crystals 5 g
Colour of crystals yellow
Melting point 119 C.
Precautions :
Use freshly prepared sodium hydroxide.
Add sodium hydroxide slowly and with constant stirring.

Preparation of 2- Naphthol Aniline or Aniline Yellow


Aim : To prepare 2- Naphthol Aniline or Aniline Yellow dye.
Chemicals :
Aniline - 5ml
Sodium nitrite 8g
Dil. HCl (5N) 20 ml
2- Naphthol 8 ml
NaOH - 3g
Starch KI paper
Theory :

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.

Detection of Carbohydrates, Proteins and Fats in the Given Foodstuff


Experiment 1
Aim : To detect the presence of carbohydrate in the given foodstuff.
Experiment
Molisch Test
Sample + 2 drops of - napthal

Observation

Inference

Reddish brown ring at junction of Carbohydrate present


2 layers

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

Charring with burnt sugar smell.

Carbohydrate present

Carbohydrate present

Carbohydrate present

Result : The given foodstuff contains carbohydrates.


Experiment 2
Aim : To detect the presence of fats / oils in the given foodstuff.
Experiment
Spot Test
Sample placed between folds of filter paper and
crushed.
Solubility Test
Sample + chloroform
Acrolein Test
Sample + potassium bisulphate + heating

Result : The given foodstuff contains fats or oil

Observation

Inference

Appearance of translucent spot

Fats or oils present

Sample dissolves

Fats or oils present

Irritating smell due to acrolein


formation

Fats or oils present

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

Result : The given foodstuff contains proteins.

Observation

Inference

Yellow or deep yellow colour

Proteins
present

Deep red colour

Proteins
present

Violet colour

Proteins
present

Blue colour on cooling

Proteins
present

Identification of Functional Groups In Given Organic Compounds


Experiment 1
Aim : To test for the presence of unsaturation in a given organic sample.
Experiment
Bromine Test
0.2g of sample dissolved in
carbon tetrachloride + 2 drops
2% bromine
Baeyers Test
Sample dissolved in acetone +
few drops of 2% alkaline
potassium permanganate.

Observation

Inference

Disappearance of orange red or


brown colour.

Presence of unsaturation

Decolourisation of pink colour.

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

Effervescence with evolution of


hydrogen gas.

Presence of alcoholic group

Yellow precipitate

Presence of alcohol with


methyl ketone group

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

Blue litmus turns red

Presence of phenolic
group

Green or reddish violet


precipitate

Presence of phenolic
group

Bromine Water Test


Sample dissolved in water + bromine
water
Cerric Ammonium Nitrate Test
Sample + water + heat + cerric ammonium
nitrate solution

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

Yellow orange precipitate

Presence of aldehyde
group

Pink colour

Presence of aldehyde
group

Yellow or red precipitate

Presence of aldehyde
group

Silver mirror on sides of test


tube

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

Blue litmus turns


red

Presence of carboxylic
acid group

Sodium hydrogen carbonate Test


Sample + pinch of NaHCO3

CO2 gas is evolved

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

Preparation of Crystals of Potash Alum


Aim : To prepare crystals of potash alum
Chemicals Required : 2.5 g of potassium sulphate, 10g of aluminium sulphate, 2-3 ml of conc.
sulphuric acid.
Theory : Potash alum is double salt of potassium sulphate and aluminium sulphate with
composition
K2SO4Al2(SO4)324(H2O). It is formed by adding equimolar mixture of hydrated aluminium
sulphate and potassium sulphate crystals with minimum amount of sulphuric acid.
K2SO4 + Al2(SO4)318(H2O) + 6 H2O K2SO4Al2(SO4)324(H2O).
Procedure :
Take 2.5 g of potassium sulphate in a 250 ml beaker and dissolve it in a minimum amount of
water by stirring with a glass rod. Heat if required.
Take 10 g of aluminium sulphate in another beaker. Add 3-4 drops of dilute sulphuric acid
to prevent hydrolysis. Then add 20 ml of water.
Heat the beaker with constant stirring.
Mix both solution in a china dish and concentrate mixture to crystallization point.
Octahedral colourless crystals are obtained. Remove mother liquor carefully.
Dry crystals between folds of filter paper and weigh them
Result :
Colour of Crystals : Colourless
Shape of Crystals : Octahedral
Weight of Crystals : .g
Precautions :
Add a few drops of dilute sulphuric acid while dissolving aluminium sulphate to prevent
hydrolysis.
Use ice cold water to wash potash alum as it is fairly soluble in water.

Preparation of Lyophobic Sol


Aim : To prepare a sample of ferric hydroxide sol..
Chemicals Required : 0.2 M ferric chloride solution, distilled water.
Theory : Hydrolysis of ferric chloride produces ferric hydroxide which undergoes agglomeration
to give particles of colloidal dimension. These particles adsorb Fe2+ ions from the solution and
acquires a positive charge which stabilizes the sol.
FeCl3 + 3H2O Fe(OH)3 + 3HCl
(red sol)
Procedure :
Pour 100 ml of distilled water in a 250 ml beaker and place it on a wire gauze for
heating.
Add 0.2 M ferric chloride solution drop wise with the help of dropper to the boiling
water. Continue heating till a deep red or a brown solution of ferric hydroxide is
obtained.
Allow contents of beaker to cool.
Filter to remove precipitate of ferric hydroxide and collect filtrate in a beaker.
The filtrate is ferric hydroxide sol.
Precautions
All glass ware should be free from impurities.
Add ferric chloride solution very slowly drop by drop to boiling water.
Use only distilled water.

Result : A sample of lyopbobic colloid of ferric hydroxide has been prepared.

Preparation of Lyophilic Sol


Aim : To prepare a sample of starch sol.
Chemicals Required : 1g starch, distilled water.
Theory : Starch forms lyophilic colloidal solution directly when mixed with hot water. Starch sol
is stable and electrically neutral.
Procedure :
Pour 100 ml of distilled water in a 250 ml beaker and place it on a wire gauze for heating.
Grind 1 g of soluble starch with a few ml of distilled water in a mortar and pestle to a
fine paste.
Pour the paste into boiling water with the help of a glass rod. Continue boiling for 2-3
minutes after addition of starch.
Allow contents of beaker to cool and filter it with the help of filter paper.
The filtrate is a starch solution.
Precautions
All glass ware should be free from impurities.
Make a thin, fine paste of starch before adding to boiling water.
Use only distilled water.
Stir the contents continuously.
Result : A sample of lyophilic colloid of starch has been prepared.

Titration of Potassium Permanganate vs Oxalic Acid

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

Titration of Potassium Permanganate vs Mohrs Salt


Aim : To determine the molarity and strength of KMnO4 by titrating it against standard solution
of Mohrs Salt.
Theory : Potassium permanganate oxidizes ferrous ammonium sulphate in acidic medium and
itself gets reduced to colourless ions.
2 KMnO4 + 3H2SO4 K2SO4 + 2MnSO4 + 3H2O + 5[O]
2FeSO4.(NH4)2SO4.6H2O + [O] Fe2(SO4)3 + 2(NH4)2SO4 + 13H2O] x 5
2 KMnO4 + 8H2SO4 + 10FeSO4.(NH4)2SO4.6H2O K2SO4 + 2MnSO4 + 5Fe2(SO4)3
+10(NH4)2SO4 + 68 H2O
Preparation of standard Solution :
1000 ml of M/20 Mohrs salt requires = 19.6 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 Mohrs salt solution and pipette out 20.0 ml of it in a washed
titration flask.
Add one test tube of dilute (4N) H2SO4 to flask, shake.
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 : (i) The molarity of KMnO4 solution is ..M.
(ii) The strength of KMnO4 solution is g/l.

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

Salt + dil. H2SO4


Salt + conc. H2SO4
Bring a rod dipped in NH4OH
near mouth of test tube

Confirmatory Test
Water extract + silver nitrate
solution

Observation
No characteristic change
Colourless gas with pungent
smell evolved
Dense white fumes are
formed.

Curdy white precipitate


soluble in excess of
NH4OH

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

Result: The given salt is NH4Cl

Experiment

To analyse

Inference

Preliminary Test

No characteristic change

Salt + dil. H2SO4

Salt + conc. H2SO4 + heat


+ copper chips

Confirmatory Test
Water extract + ferrous
sulphate + conc. H2SO4
along sides of test tube

Experiment
Nature of the salt
Original solution +

Reddish brown vapours


evolve which intensify with
copper chips

Reddish brown ring is formed


at junction of two layers

Absence of
CO32-, S2-, SO32-, NO2indicated
NO3- indicated

NO3- confirmed

Observation
White crystalline, dissolves
in water.

Inference

No characteristic change

Absence of NH4+ indicated

NaOH + heat

White precipitate forms


Pb2+ indicated
Original solution +
Dilute HCl
Boil white precipitate Precipitate dissolves. Divide
into 2 parts
with water
Yellow precipitate
Pb2+ confirmed
1 part of solution +
potassium chromate
Yellow precipitate
Pb2+ confirmed
1 part of solution +
potassium iodide

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

Salt + dil. H2SO4

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-

Salt + BaCl2 solution

Confirmatory Test
Water extract + lead
acetate

in dilute HCl.

Indicated
SO42- indicated

White precipitate is formed

SO42- confirmed

Result: The given salt is Al2 (SO4)3


4. Aim: To analyse the presence of anion and cation in the given salt sample.

Experiment
Nature of the salt
Original solution +

Observation
White crystalline, dissolves
in water.

Inference

No characteristic change

Absence of NH4+

NaOH + heat

Original solution +Dilute HCl


Original solution +
Dilute HCl + H2S gas
Original solution + NH4Cl(s) +
NH4OH

indicated
No characteristic change

Absence of Group I
indicated

No characteristic change

Absence of Group II
indicated

Gelatinous white precipitate.


Dissolve in dilute HCl and
divide

Al3+ indicated

Into 2 parts

Part 1 + NaOH
Part 2 + blue litmus+ NH4OH
dropwise

White precipitate soluble in


excess
NaOH.
Blue Lake (Blue precipitate
floating in colourless solution)

Al3+ confirmed
Al3+ confirmed

Experiment
Nature of the salt
Original solution +

Observation
White crystalline, dissolves
in water.

Inference

No characteristic change

Absence of NH4+ indicated

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

Original solution + NH4Cl(s) +


NH4OH

No characteristic change

Absence of Group III


indicated

Original solution + NH4Cl(s)


+ NH4OH + H2S gas

Part 1 + NaOH
Part 2 + K4[Fe(CN)6]

Experiment
Preliminary Test

Salt + dil. H2SO4

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

White precipitate insoluble


in dilute HCl.

White precipitate is formed

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

Absence of NH4+ indicated

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

Result: The given salt is ZnSO4


5. Aim: To analyse the presence of anion and cation in the given salt sample.

Absence of Group IV

Original solution + NH4Cl(s)


+ NH4OH + H2S gas

Group V indicated

Original solution + NH4Cl(s)

White precipitate
Dissolve precipitate in acetic
acid and divide into 3 parts
Yellow precipitate

+ NH4OH + (NH4)2CO3

Part 1 + potassium chromate

Experiment
Preliminary Test

indicated

No characteristic change

Observation
No characteristic change

Inference
Absence of
CO32-, S2-, SO32-, NO2indicated

Curdy white precipitate


soluble in excess of
NH4OH

Cl- confirmed

Salt + dil. H2SO4


Salt + conc. H2SO4
Bring a rod dipped in NH4OH
near mouth of test tube

Confirmatory Test
Water extract + silver nitrate
solution

Ba2+ confirmed

Result: The given salt is BaCl2

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

Salt + dil. H2SO4

No characteristic change
Salt + conc. H2SO4

Absence of

No characteristic change
Salt + BaCl2 solution
Salt + conc. HNO3 + heat
+ ammonium molybdate

Canary yellow precipitate


formed

Cl-, Br-, I-, NO3-, CH3COO-,


C2O4Indicated
Absence of SO42- indicated
PO43- confirmed

Result: The given salt is Mg3(PO4)2

Experiment
Nature of the salt
Original solution +

Observation
White crystalline, dissolves
in water.

Inference

No characteristic change

Absence of NH4+ indicated

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

Original solution + NH4Cl(s) + NH4OH

indicated
Absence of Group III

No characteristic change

Original solution + NH4Cl(s)


+ NH4OH + H2S gas

indicated
Absence of Group IV

No characteristic change

Original solution + NH4Cl(s)


+ NH4OH + (NH4)2CO3

indicated

No characteristic change

indicated
Absence of Group V
indicated

Original solution + NH4Cl(s)


+ NH4OH + (NH4)2HPO4

White precipitate on
scratching
Inner side of test tube

Mg2+ confirmed