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 Observation Inference

Molisch Test
Sample + 2 drops of - napthal Reddish brown ring at junction of Carbohydrate present
2 layers
Fehling’s Test
Sample + Fehling’s solution + Yellow or red precipitate Carbohydrate present
warm in water bath.
Benedict’s Test
Sample + Benedict’s solution + Red precipitate Carbohydrate present
warm in water bath.

Conc. H2SO4 Test

Sample + Conc. H2SO4 Charring with burnt sugar smell. Carbohydrate present

Result : The given foodstuff contains carbohydrates.

Experiment 2

Aim : To detect the presence of fats / oils in the given foodstuff.

Experiment Observation Inference

Spot Test
Sample placed between folds of filter paper and Appearance of translucent spot Fats or oils present
crushed.

Solubility Test
Sample + chloroform Sample dissolves Fats or oils present
Acrolein Test
Sample + potassium bisulphate + heating Irritating smell due to acrolein Fats or oils present
formation

Result : The given foodstuff contains fats or oil

Experiment 3

Aim : To detect the presence of protein in the given foodstuff.

Experiment Observation Inference

xanthproteic Test
Sample + few ml of conc. HNO3 Yellow or deep yellow colour Proteins
Shake and leave undisturbed. present

Millon’s Test
Sample + few drops of mercuric nitrate+ Deep red colour Proteins
1 drop dil. HCl + Boil , Cool + 1drop NaNO3 present
+ Heat mixture
Biuret Test
Sample + 10% NaOH + dil. CuSO4 Violet colour Proteins
present
Ninhydrin Test
Sample + 0.1% ninhydrin solution + boil for 1 Blue colour on cooling Proteins
minute present

Result : The given foodstuff contains proteins.

Identification of Functional Groups In Given Organic Compounds

Experiment 1

Aim : To test for the presence of unsaturation in a given organic sample.

Experiment Observation Inference

Bromine Test
0.2g of sample dissolved in Disappearance of orange red or Presence of unsaturation
carbon tetrachloride + 2 drops brown colour.
2% bromine
Baeyer’s Test
Sample dissolved in acetone + Decolourisation of pink colour. Presence of unsaturation
few drops of 2% alkaline
potassium permanganate.

Experiment 2

Aim : To test for the presence of alcoholic group in a given organic sample.

Experiment Observation Inference

Ester Test
Sample + few drops of acetic acid + Pleasant smell Ester present
Conc. H2SO4
Warm in a water bath.
Sample + small piece of Na metal Effervescence with evolution of Presence of alcoholic group
hydrogen gas.
Iodoform Test
Sample + NaOH solution + solid I2 Yellow precipitate Presence of alcohol with
+ warm methyl ketone group

Experiment 3

Aim : To test for the presence of phenolic group in organic sample

Experiment Observation Inference

Litmus Test
Sample + blue litmus Blue litmus turns red Presence of phenolic
group
FeCl3 Test
Sample + small amount of FeCl3 Green or reddish violet Presence of phenolic
precipitate group
Bromine Water Test
Sample dissolved in water + bromine White precipitate Presence of phenolic
water group
Cerric Ammonium Nitrate Test
Sample + water + heat + cerric ammonium Green or brown Presence of phenolic
nitrate solution precipitate group

Experiment 4

Aim : To test for the presence of aldehyde group in organic sample.

Experiment Observation Inference

2,4 – Dinitrophenyl hydrazine
Test Yellow orange precipitate Presence of aldehyde
2,4 – DNP + sample group
Schiff’s Test
Sample + Schiffs Reagent Pink colour Presence of aldehyde
group
Fehling’s Test
Sample + Fehling’s solution + Yellow or red precipitate Presence of aldehyde
warm in water bath group
Tollen’s Test
Sample + Tollen’s solution + Silver mirror on sides of test Presence of aldehyde
warm in water bath tube group

Experiment 5

Aim : To test for the presence of carboxylic acid group in organic sample.

Experiment Observation Inference

Litmus Test
Sample + blue litmus Blue litmus turns Presence of carboxylic
red 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 Red or Yellow Presence of carboxylic
NH3. Cool and add neutral FeCl3 precipitate 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)3·24(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)3·18(H2O) + 6 H2O → K2SO4Al2(SO4)3·24(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 60°C and itself gets reduced to colourless ions.
2 KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5[O]
COOH 60°C
| + [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 60°C
 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 Volume of

KMnO4 used (ml)
Initial Final
1.
2.
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 Mohr’s 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 Mohr’s 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 Mohr’s salt = M/20
Volume of Mohr’s salt = 10 ml
 S No. Burette Reading Volume of
KMnO4 used (ml)
Initial Final
1.
2.

Calculations
(i) KMnO4 = Mohr’s 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 Observation Inference To analyse
 Nature of the salt White crystalline, dissolves the presence
in water.
of anion and
 Original solution Gas with pungent smell of ammonia NH4+ indicated
+ evolved. cation in the
NaOH + heat Forms dense white fumes with HCl given salt
sample.
 Original solution Brown precipitate NH4+
+ confirmed
Nessler’s reagent

Experiment Observation Inference

Preliminary Test No characteristic change Absence of
 Salt + dil. H2SO4 CO32-, S2-, SO32-, NO2-
 Salt + conc. H2SO4 Colourless gas with pungent indicated
smell evolved
Bring a rod dipped in NH4OH Dense white fumes are

near mouth of test tube formed. Cl- indicated

Confirmatory Test
 Water extract + silver nitrate Curdy white precipitate Cl- confirmed
solution soluble in excess of
NH4OH

Result: The given salt is NH4Cl

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

Experiment Observation Inference

 Preliminary Test Absence of
 Salt + dil. H2SO4 No characteristic change CO32-, S2-, SO32-, NO2-
indicated
Reddish brown vapours NO3- indicated
 Salt + conc. H2SO4 + heat evolve which intensify with
+ copper chips copper chips

Confirmatory Test
 Water extract + ferrous Reddish brown ring is formed NO3- confirmed
sulphate + conc. H2SO4 at junction of two layers
along sides of test tube

Experiment Observation Inference

 Nature of the salt White crystalline, dissolves
in water.
 Original solution + No characteristic change Absence of NH4+ indicated
NaOH + heat
 Original solution + White precipitate forms Pb2+ indicated Result:
Dilute HCl The
 Boil white precipitate Precipitate dissolves. Divide given salt
with water into 2 parts is
 1 part of solution + Yellow precipitate Pb2+ confirmed Pb(NO3)2
potassium chromate
 1 part of solution + Yellow precipitate Pb2+ confirmed
potassium iodide

3. Aim: To analyse the presence of anion and cation in the given salt sample.
Experiment Observation Inference
Preliminary Test Absence of
 Salt + dil. H2SO4 No characteristic change CO32-, S2-, SO32-, NO2-
indicated
No characteristic change
 Salt + conc. H2SO4 Absence of
Cl-, Br-, I-, NO3-, CH3COO-,
White precipitate insoluble C2O4-
  Salt + BaCl2 solution in dilute HCl. Indicated
SO42- indicated

Confirmatory Test
 Water extract + lead White precipitate is formed SO42- confirmed
acetate

Result: The given salt is Al2 (SO4)3

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

Experiment Observation Inference

 Nature of the salt White crystalline, dissolves
in water.
 Original solution + No characteristic change Absence of NH4+
NaOH + heat indicated

 Original solution +Dilute HCl No characteristic change Absence of Group I

indicated
 Original solution + No characteristic change Absence of Group II
Dilute HCl + H2S gas
indicated
 Original solution + NH4Cl(s) +
NH4OH Gelatinous white precipitate. Al3+ indicated
Dissolve in dilute HCl and
divide
Into 2 parts
 Part 1 + NaOH White precipitate soluble in Al3+ confirmed
excess
NaOH.
 Part 2 + blue litmus+ NH4OH Blue Lake (Blue precipitate Al3+ confirmed
dropwise floating in colourless solution)
 Experiment Observation Inference
 Nature of the salt White crystalline, dissolves
in water.
 Original solution + No characteristic change Absence of NH4+ indicated
NaOH + heat

 Original solution + No characteristic change Absence of Group I

Dilute HCl indicated

 Original solution +
Dilute HCl + H2S gas 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 Zn2+ indicated
White precipitate
Dissolve precipitate in HCl.
Boil off H2S. Divide into 2
parts
 Part 1 + NaOH White precipitate soluble in Zn2+ confirmed
excess NaOH.
Part 2 + K4[Fe(CN)6] White or bluish white Zn2+ confirmed
precipitate.

Experiment Observation Inference

Preliminary Test Absence of
 Salt + dil. H2SO4 No characteristic change CO32-, S2-, SO32-, NO2-
indicated
No characteristic change
 Salt + conc. H2SO4 Absence of
Cl-, Br-, I-, NO3-, CH3COO-,
White precipitate insoluble C2O4-
 Salt + BaCl2 solution in dilute HCl. Indicated
SO42- indicated

Confirmatory Test
 Water extract + lead White precipitate is formed SO42- confirmed
acetate
 Experiment
 Nature of the salt
 Original solution +
NaOH + heat
 Original solution +
Dilute HCl
 Original solution +
Dilute HCl + H2S gas
 Original solution + NH4Cl(s) +
NH4OH
Result: The given salt is ZnSO4
5. Aim: To analyse the presence of anion and cation in the given salt sample.
Observation Inference
White crystalline, dissolves
in water.
No characteristic change Absence of NH4+ indicated
Absence of Group I
No characteristic change indicated
Absence of Group II
No characteristic change indicated
Absence of Group III
No characteristic change indicated
 Absence of Group IV
 Original solution + NH4Cl(s)
+ NH4OH + H2S gas indicated
No characteristic change

Group V indicated
 Original solution + NH4Cl(s) White precipitate
+ NH4OH + (NH4)2CO3 Dissolve precipitate in acetic
acid and divide into 3 parts
 Part 1 + potassium chromate Yellow precipitate Ba2+ confirmed

Experiment Observation Inference

Preliminary Test No characteristic change Absence of
 Salt + dil. H2SO4 CO32-, S2-, SO32-, NO2-
 Salt + conc. H2SO4 indicated
 Bring a rod dipped in NH4OH
near mouth of test tube

Confirmatory Test
 Water extract + silver nitrate Curdy white precipitate Cl- confirmed
solution soluble in excess of
NH4OH

Result: The given salt is BaCl2

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

Observation Inference
Experiment

Preliminary Test Absence of

 Salt + dil. H2SO4 No characteristic change CO32-, S2-, SO32-, NO2-
indicated
No characteristic change
 Salt + conc. H2SO4 Absence of

 Salt + BaCl2 solution
 Salt + conc. HNO3 + heat
+ ammonium molybdate
Result: The given salt is Mg3(PO4)2
Experiment
 Nature of the salt
 Original solution +
NaOH + heat
 Original solution +
Dilute HCl
 Original solution +
Dilute HCl + H2S gas
 Original solution + NH4Cl(s) + NH4OH
 Original solution + NH4Cl(s)
+ NH4OH + H2S gas
 Original solution + NH4Cl(s)
+ NH4OH + (NH4)2CO3
 Original solution + NH4Cl(s)
+ NH4OH + (NH4)2HPO4
Cl-, Br-, I-, NO3-, CH3COO-,
C2O4-
No characteristic change Indicated
Canary yellow precipitate Absence of SO42- indicated
formed
PO43- confirmed
Observation Inference
White crystalline, dissolves
in water.
No characteristic change Absence of NH4+ indicated
Absence of Group I
No characteristic change indicated
Absence of Group II
No characteristic change indicated
Absence of Group III
No characteristic change indicated
Absence of Group IV
indicated
No characteristic change
Absence of Group V
No characteristic change
indicated
Mg2+ confirmed
White precipitate on
scratching
Inner side of test tube