Quantitative and Content Based Experiments Record

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QUANTITATIVE & CONTENT

BASED EXPERIMENTS

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Calculation of weight of Ferrous Ammonium sulphate for the preparation of standard
solution of 100ml of M/20 (Mohr’s salt solution):

Molarity of Mohr’s salt solution = Weight of Mohr’s salt x 1000 0


Molar mass of Mohr’s salt x 100

Weight of Mohr’s salt = Molarity of Mohr’s salt solution x Mol.mass of Mohr’s salt x 100
1000

Weight of Mohr’s salt = 1/20 x 392 x 1/10 = 1.96g

Mohr’s salt solution Vs Potassium permanganate solution


Indicator – Potassium permanganate solution (self)

Volume of
S.No Volume of Burette reading (ml) KMnO4
FAS solution Initial Final Solution (ml) Concordant
(ml) value

1. 20 0 ----------
---------- ----------
2. 20 0 ----------

Calculation:
V1M1a = V2M2b
Volume of Molarity of Volume of Molarity of
Mohr’s salt x Mohr’s salt x 1 = KMnO4 x KMnO4 x 5
Solution Solution Solution Solution

20 ml x ----------------M x 1 = -------------- ml x M x 5
M KMnO4 = 20ml x ------------M x 1
------------ ml x M x 5
= -------------------M
Strength of Molarity of x Molar mass of x Volume in litre
KMnO4 solution = KMnO4 solution KMnO4 solution

= -----------M x 158 x 1lit

= ----------- g/lit

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EXPT. NO: 1 1

DATE: 1

ESTIMATION OF POTASSIUM PERMANGANATE SOLUTION


AIM:
To prepare a standard solution of M/20 Ferrous Ammonium sulphate solution and to
determine the molarity and weight/litre of the given Potassium permanganate solution.

MATERIALS REQUIRED:
Burette, Pipette, Standard flask, Conical Flask, Funnel, Burette stand, Glazed tile,
Potassium permanganate solution, Ferrous Ammonium sulphate crystals and dilute Sulphuric
acid.

THEORY:
It is a Redox reaction in which Potassium permanganate is the oxidising agent and
gets reduced by gaining 5 electrons per molecule and Ferrous Ammonium sulphate is the
reducing agent and undergoes oxidation by losing 1 electron per molecule.

MnO4- + 8H+ + 5e-  Mn2+ + 4H2O


5Fe2+  5Fe3+ + 5e-
MnO4 - + +
8H + 5Fe 2+
 5Fe3+ + Mn2+ + 4H2O

SIMPLE PROCEDURE:

1. Burette solution: Potassium permanganate solution


2. Pipette Solution: 20ml of standard FAS
3. Condition: 20ml dilute Sulphuric acid added to conical flask
4. Temperature - room temperature.
5. Indicator: Potassium permanganate (Self indicator)
6. End point: Appearance of pale permanent pink colour

RESULT:

(i) Molarity of the given Potassium permanganate solution = ------------------------.

(ii) Strength of given Potassium permanganate solution = -------------------- g/lit.

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Calculation of weight of Oxalic acid for the preparation of M/50 standard solution in
100ml :

Molarity of Oxalic acid solution = Weight of Oxalic acid x 1000 0


Molar mass of Oxalic acid x 100
Weight of Oxalic acid = Molarity of Oxalic acid solution x Molarmass of Oxalic acid x 100
1000
Weight of Oxalic acid = 1/50 x 126 x 1/10 = 0.252 g

Oxalic acid solution Vs Potassium permanganate solution


Indicator – Potassium permanganate solution (self)

Burette reading (ml) Volume of


Volume of Oxalic acid KMnO4 Concordant
S.No solution (ml) Initial Final Solution (ml) value

1. 20 0 ---------- ----------
----------
2. 20 0 ---------- ----------

Calculation:
V1M1a = V2M2b
Volume of Molarity of Volume of Molarity of
Oxalic acid x Oxalic acid x 2 = KMnO4 x KMnO4 x 5
solution solution Solution Solution

20 ml X ----------------M x 2 = -------------- ml x M x 5
M KMnO4 = 20ml x ------------M x 2
-------------- ml x M x 5
= -------------------M

Strength of Molarity of x Molar mass of x Volume in litre


KMnO4 solution = KMnO4 solution KMnO4 solution

= -----------M x 158 x 1lit

= ----------- g/lit

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EXPT. NO: 2 1

DATE: 1
ESTIMATION OF POTASSIUM PERMANGANATE SOLUTION
AIM:

To prepare a standard solution of M/50 Oxalic acid solution and to determine the
molarity and weight/litre of the given Potassium permanganate solution.

MATERIALS REQUIRED:
Burette, Pipette, Standard flask, Conical Flask, Funnel, Burette stand, Glazed tile,
Wire gauze, Potassium permanganate solution, Oxalic acid crystals and dilute Sulphuric acid.

THEORY:
It is a Redox reaction in which Potassium permanganate is the oxidising agent and
gets reduced by gaining 5 electrons per molecule and Oxalic acid is the reducing agent and
undergoes oxidation by losing 2 electron per molecule.

(MnO4- + 8H+ + 5e-  Mn2+ + 4H2O)2


(C2O42-  2CO2 + 2e-) 5
2MnO4 + 16H + 5 C2O42-  2Mn2+ + 10CO2 + 8H2O
- +

SIMPLE PROCEDURE:

1. Burette solution: Potassium permanganate solution


2. Pipette Solution: 20ml of standard Oxalic acid
3. Condition: 20ml dilute Sulphuric acid added to conical flask
4. Temperature - 40 ⁰C to 60 ⁰C.
5. Indicator: Potassium permanganate (Self indicator)
6. End point: Appearance of pale permanent pink colour

RESULT:

(i) Molarity of the given Potassium permanganate solution = -------------------------.

(ii) Strength of given Potassium permanganate solution = --------------------g/lit.

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S.NO Colour of the Distance travelled Distance travelled Retention factor
. dye by by value (Rf)
solute (cm) solvent(cm)
1. Red

2. Blue

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EXPT. NO:____3______

DATE : ______________

PAPER CHROMATOGRAPHY (I)

AIM:

To separate a mixture of dyes by paper chromatography and to compare their


retention factor value (Rf) and to attach the chromatogram.

APPARATUS REQUIRED:

Boiling tube, filter paper, fine capillary tube.

PROCEDURE:

Take a filter paper strip and draw a line at the centre with a pencil from one end to
another. Draw another line lengthwise from the centre of the paper. With the help of a
capillary tube, place a drop of mixture of dyes and let it dry in air. Place another drop on the
same spot and let it dry. Repeat two times so that the spot is rich in mixture. Suspend the
filter paper vertically in a boiling tube containing water as a solvent and place it undisturbed
for some time. Note the rising solvent. Take the filter paper out of the boiling tube, mark the
distance travelled by the solvent. Dry the filter paper. Notice the chromatogram which shows
two spots, a top green spot and a lower red spot of the dyes. Measure the distance travelled by
the dyes and the solvent from the starting line and calculate Rf.

Retention factor (Rf) = Distance travelled by solute


Distance travelled by solvent

RESULT:

Retention factor value of green dye = _________________

Retention factor value of red dye = _________________

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S.NO. Volume of Volume of Total Volume Time (s) 1/t (s-1)
Na2S2O3 (ml) water(ml) volume(ml) of HCl
(ml)

1. 10 40 50 10

2. 20 30 50 10

3. 30 20 50 10

4. 40 10 50 10

5. 50 0 50 10

1/t (S-1)

Volume of sodium thiosulphate (ml)

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EXPT. NO: _____4_____

DATE: ______________

EFFECT OF CONCENTRATION ON RATE OF REACTION

AIM:

To study the effect of concentration on the rate of the reaction between sodium
thiosulphate and hydrochloric acid.

MATERIALS REQUIRED:

Measuring cylinders (100ml & 10ml), stop clock and conical flask, 0.1M sodium
thiosulphate, 1M hydrochloric acid.

THEORY:

According to the law of mass action, rate of reaction is directly proportional to the
product of the molar concentrations of the reactants. That is the rate of the reaction increases
with the increase in the concentration of the reactants. Effect of concentration of the reactant
on the rate of the reaction can be studied easily by the reaction between sodium thiosulphate
and hydrochloric acid.

Na2S2O3 + 2HCl S(s) + 2NaCl(aq) + SO2 (g) + H2O(l)

The insoluble sulphur formed during the reaction gives a milky appearance that is it
makes the solution turbid. Rate of reaction can be studied by measuring the time taken to
produce enough sulphur to make the cross-mark invisible on a paper kept under the conical
flask in which the reaction is carried out.

PROCEDURE:

Wash a conical flask with water. Add 10ml of 0.1M sodium thiosulphate, 40ml of
water such that the total volume is 50ml. Take 10ml of 1M hydrochloric acid in a test tube
and add it to the conical flask. Shake the contents and place the flask on a paper with a cross
marked on it. Observe the mark. Note the time taken for the mark to become invisible. Repeat
the experiment with 20, 30, 40, and 50ml of sodium thiosulphate. Plot the graph between
volume(ml) of sodium thiosulphate on the X axis and 1/t (s-1) on the Y axis.

RESULT:

From the graph it is clear that 1/t is directly proportional to the concentration of
sodium thiosulphate but 1/t is a direct measure of the rate of the reaction. Hence the rate of
reaction between sodium thiosulphate and hydrochloric acid is directly proportional to the
volume of sodium thiosulphate solution taken. Hence the rate of reaction is directly
proportional to the concentration of sodium thiosulphate which is one of the reactants.

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EXPT. No. : ___5____

DATE : _____________
PREPARATION OF 2-NAPHTHOL ANILINE OR β- NAPHTHOL ANILINE DYE
AIM:
To prepare 2-Naphthol, Anililne or β-Naphthol Aniline dye.
APPARATUS REQUIRED:
100mL conical flask, measuring cylinder, 100mLbeaker, thermometer, funnel, filter
paper.
CHEMICALS REQUIRED:
Aniline, Concentrated HCl, Sodium nitrite, β-naphthol, 10% NaOH solution, distilled
water, sodium chloride
THEORY:
β-Naphthol aniline dye is prepared by coupling reaction of Benzene diazonium
chloride with alkaline solution of β-naphthol at a temperature below 5⁰C. Benzene diazonium
chloride required for the reaction can be obtained by the diazotisation of Anililne with
Nitrous acid at 0-5⁰C.

PROCEDURE:
Dissolve 5mL Aniline in a mixture of 10ml concentrated HCl and 10mL water in a
conical flask. Cool the solution to 5⁰C. In a test tube dissolve 8g NaNO2 in 20mL of water.
Cool this in an ice bath. Diazotise Aniline or add cooled solution of NaNO 2 to cooled
solution of aniline. Shake the solution for some time. Add some ice to the reaction mixture.
This is benzene diazonium chloride solution. Now take 25mL Sodium Hydroxide solution in
a beaker and add about 8g of β-Naphthol to it. Stir to dissolve β-Naphthol and let it cool to
5⁰C. Add the diazonium salt solution very slowly to β-Naphthol solution with stirring. A red
coloured solid dye separates out. Allow the mixture to stand for 30 minutes in a beaker
containing ice. Filter the solid and wash well with water. Dry between the folds of filter
paper. Re-crystallize a small amount by dissolving in acetic acid.

RESULT:
Weight of crystal =
Colour of the crystal – Red

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EXPT. NO:_____6_____

DATE: ______________

PREPARATION OF LYOPHILIC SOL

AIM:

To prepare colloidal starch.

MATERIALS REQUIRED:

Beaker, glass rod, funnel, tripod stand, wire gauze, burner, soluble starch(1g) and distilled
water.

THEORY:

Starch forms a lyophilic sol when water is used as the dispersion medium. The formation of
sol is accelerated by heating. The starch sol can be prepared by heating starch and water at
about 100°C. It is quite stable and is not affected by the presence of any electrolytic impurity.

PROCEDURE:

Take 1g of starch and add a few millilitres of distilled water in a 100ml beaker. Grind the
starch to make a thin paste and transfer into a 250ml beaker containing 100ml of distilled
water. Heat the beaker till the water starts boiling and continue boiling for 3-4 minutes.
Allow to cool. Filter the contents of the beaker through a filter paper, fixed in a funnel.

PRECAUTIONS:

1. Apparatus must be clean.


2. Starch must be made into a fine paste before adding to boiling water.
3. Constant stirring of contents is necessary during preparation.

RESULT:

Starch sol was prepared.

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EXPT. NO:_____7_____

DATE: ______________

PREPARATION OF LYOPHOBIC SOL

AIM:

To prepare colloidal sol of Ferric hydroxide.

MATERIALS REQUIRED:

Beaker, conical flask, glass rod, tripod stand, wire gauze, burner, 2% Ferric chloride prepared
by dissolving 2g of pure Ferric chloride in 100ml of distilled water.

THEORY:

Ferric hydroxide is a lyophobic sol. It is prepared by the hydrolysis of ferric chloride in


boiling distilled water. The reaction that takes place can be represented as

FeCl3(aq) + 3H2O Fe(OH)3+ 3HCl

The hydrolysis produces insoluble ferric hydroxide particles which undergo peptization and
yield particles of colloidal dimensions. The Fe3+ ions are adsorbed from the solution to form
the colloidal particles and this gives a positive charge to the colloidal particles. The stability
of the sol is due to the charge on the sol particles. Hydrochloric acid which is produced
during hydrolysis tries to destabilize the sol and hence it must be removed.

PROCEDURE:

Take a clean conical flask. Add 100ml of distilled water and heat it to boil. Add ferric
chloride solution drop wise to the boiling water. Continue heating until a deep red or brown
solution of ferric hydroxide is obtained. Replace the water lost by evaporation during boiling
at regular intervals. Keep the contents of the conical flask undisturbed for sometime at room
temperature.

RESULT:

Ferric hydroxide sol was prepared.

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EXPT. NO:____8______

DATE: ______________

PREPARATION OF POTSH ALUM CRYSTALS

AIM:

To prepare a pure sample of Potash alum. (K2SO4. Al2(SO4)3.24H2O)

APPARATUS REQUIRED:

Two beakers. China dish, funnel, tripod stand and wire gauze.

CHEMICALS REQUIRED:

Potassium sulphate, Aluminium sulphate and dilute Sulphuric acid.

THEORY:

It is prepared by dissolving an equimolar solution of hydrated aluminium sulphate and


potassium sulphate in a minimum amount of water containing a little sulphuric acid, then
subjecting the resultant solution to crystallization when octahedral crystals separate out.

K2SO4+ Al2(SO4)3.18H2O + 6H2O K2SO4. Al2(SO4)3.24H2O

PROCEDURE:

Take a 250ml beaker and wash it with distilled water. Transfer 2.5g of potassium sulphate
crystals to it. Add about 20ml of water and stir to dissolve the crystals, warm if required.
Take another beaker, wash it and transfer 10g of aluminium sulphate crystals to it. Add about
20ml of water and 1ml of dilute sulphuric acid to prevent hydrolysis of aluminium sulphate.
Heat for 5 minutes. If solution is turbid, filter it. Mix the two solutions in a china dish and
heat it to the crystallization point. Allow it to cool slowly. Crystals of potash alum separate
out. Wash the crystals and dry them.

RESULT:

Weight of crystals = __________ g.

Colour of crystals is white.

Shape of the crystals is octahedral.

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EXPT. NO: ___9_______

DATE: ______________

FOOD TEST

AIM:

To identify the presence of proteins, carbohydrates and fats in the given compounds.

I TEST FOR CARBOHYDRATES:

EXPERIMENT OBSERVATION INFERENCE


1. MOLISCH TEST: Violet ring is formed. Presence of carbohydrate.
To the substance add Molisch Red precipitate
Violet ring is formed
is Presence
Presence
ofof
carbohydrate.
Carbohydrate
reagent and concentrated obtained. Presence of carbohydrate.
sulphuric acid along the sides of A shining silver mirror is Presence of carbohydrate.
the test tube. formed.
Red precipitate is formed.
2. BENEDICT’S TEST:
To the substance add Red Precipitate is obtained Presence of Carbohydrate
Benedict’s reagent and heat.

3. TOLLEN’S TEST: A shiny silver mirror is Presence of Carbohydrate


To the substance add Tollen’s formed
reagent and heat.

4. FEHLING’S TEST:
To the substance add Fehling Red precipitate is formed Presence of Carbohydrate
A and B and heat.

II TEST FOR OILS AND FATS:

EXPERIMENT OBSERVATION INFERENCE


1. SOLUBILITY:
To the substance add Soluble in chloroform. Presence of oils and fats.
chloroform.

2. ACROLEIN TEST:
To the substance add Pungent irritating odour. Presence of oils and fats.
potassium bisulphate and heat.

3. TRANSLUCENT SPOT Appearance of translucent


TEST: or greasy spot. Presence of oils and fats.
Press a little of the substance
in the folds of a filter paper.

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III TEST FOR PROTEINS:

EXPERIMENT OBSERVATION INFERENCE


1. BIURET TEST:
To the substance add 2ml of Bluish violet colour is Presence of proteins.
sodium hydroxide and 4 - 5 obtained.
drops of copper sulphate
solution.

2. MILLON’S TEST:
To the substance add Millon’s White precipitate is Presence of proteins
reagent. obtained which becomes
brick red on heating.

3. NINHYDRIN TEST:
To the substance add 2ml of Intense blue colouration is Presence of proteins.
Ninhydrin solution and heat. obtained.

RESULT:

The given sample is identified as ----------------, -------------------, ----------------.

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EXPT. NO: ___10_______

DATE: ______________

TEST FOR FUNCTIONAL GROUPS

AIM:

To identify the functional group present in the given organic compound.

I. TESTS FOR UNSATURATION:

EXPERIMENT OBSERVATION INFERENCE


1.BROMINE WATER TEST:
To the compound add a drop Disappearance of brown Presence of unsaturation.
of bromine water and shake. colour of bromine.

2.ALKALINE POTASSIUM
PERMANGANATE TEST:
Add alkaline potassium Pink colour decolourises Presence of unsaturation.
permanganate (Baeyer’s with or without the
reagent) to the compound. formation of brown
coloured precipitate of
manganese dioxide.

3. SOOTY FLAME TEST:


Take a small amount of the Substance burns with a Presence of unsaturation.
compound in a nickel spatula yellow flame with lots of
and heat. black smoke.

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II TESTS FOR ALCOHOLS:

EXPERIMENT OBSERVATION INFERENCE


1. SODIUM METAL TEST:
Add a piece of dry sodium Brisk effervescence due Presence of alcoholic group.
metal to the compound to liberation of hydrogen
gas is seen.

2. ESTERIFICATION TEST:
To the compound of add A fruity smell is occurred Presence of alcoholic group.
acetic acid, 2 drops of due to the formation of
concentrated sulphuric acid, warm an aster.
the solution and pour into to a
beaker containing water.

3. CERIC AMMONIUM
NITRATE TEST:
To the compound add a few Appearance of red or Presence of alcoholic group.
drops of ceric ammonium nitrate pink colouration.
reagent and shake well.

RESULT:
The given sample contains ----------------------- functional group.

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III. TESTS FOR PHENOL:

EXPERIMENT OBSERVATION INFERENCE


1. LITMUS TEST:
To the compound add litmus Blue litmus turns red. Presence of phenolic group.
solution.

2. NEUTRAL FERRIC
CHLORIDE TEST: Violet colour is produced on Presence of phenolic group.
Add neutral ferric chloride to dilution.
the compound.

3. LIBERMANN’S TEST:
To the compound dissolved in Deep green colour appears. Presence of phenolic group.
conc. Sulphuric acid and 2-3 On dilution red colour
crystals of Sodium Nitrate. appears. On adding sodium
Heat gently and allow to cool. hydroxide blue or green
Dilute the contents and then colour appears.
add an excess of sodium
hydroxide solution.

4. PHTHALIC
ANHYDRIDE TEST:
To the compound add a few Pink colour is obtained. Presence of phenolic group.
crystals of phthalic anhydride
and concentrated Sulphuric
acid and heat strongly. Pour
into another test tube
containing Sodium hydroxide
solution.

RESULT:

The given sample contains ----------------------- functional group.

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IV. TESTS FOR ALDEHYDE:

EXPERIMENT OBSERVATION INFERENCE


2,4-DNP TEST:
Take 1 ml of aqueous or alcoholic
solution of the given compound and A yellowish orange May be presence of
add few drops of 2,4- precipitate is obtained aldehyde or ketone
dinitrophenylhydrazine. Boil the
mixture and cool

1. TOLLEN’S REAGENT TEST:


To the compound add litmus solution. A shiny silver mirror Presence of aldehyde.
is obtained
2. FEHLING TEST:
To the compound add Fehling’s A and Appearance of red
B solution and warm. precipitate with the Presence of aldehyde.
formation of cuprous
oxide.

RESULT:

The given sample contains ----------------------- functional group.

V. TESTS FOR KETONE:

EXPERIMENT OBSERVATION INFERENCE


2,4-DNP TEST:
Take 1 ml of aqueous or alcoholic
solution of the given compound and A yellowish orange May be presence of
add few drops of 2,4- precipitate is obtained aldehyde or ketone
dinitrophenylhydrazine. Boil the
mixture and cool

1. SODIUM NITROPRUSSIDE
TEST: Red coloured solution Presence of ketone.
To the compound add sodium is obtained
nitroprusside solution shake and add
sodium hydroxide drop wise.

RESULT:

The given sample contains ----------------------- functional group.

20
VI. TESTS FOR CARBOXYLIC ACID:

EXPERIMENT OBSERVATION INFERENCE


1. LITMUS TEST:
To the compound add blue Blue litmus turns red. Presence of carboxylic acid.
litmus solution.

2.SODIUM BICARBONATE
TEST:
To the compound add sodium Brisk effervescence due to Presence of carboxylic acid.
bicarbonate solution. the evolution of carbon
dioxide.
3.ESTERIFICATION TEST:
To the compound add ethanol, Fruity smell is observed Presence of carboxylic acid.
2 drops of sulphuric acid and with the formation of an
warm. Pour into a beaker ester.
containing water.

RESULT:

The given sample contains ----------------------- functional group.

21
VII. TESTS FOR AMINE:

EXPERIMENT OBSERVATION INFERENCE


1.SOLUBILITY:
To thegiven compound add add The compound dissolves. Presence of amino group.
2-3 ml of dilute hydrochloric
acid.

2. LITMUS TEST:
Place a drop of the given liquid Red litmus turns blue. Presence of amino group.
on moist litmus paper.

3.CARBYLAMINE TEST:
Take potassium hydroxide
solution and add 2 ml of ethyl
alcohol, warm and then add a Unpleasant odour with Presence of amino group.
few ml of chloroform and a the formation of
small amount of the compound isocyanide.
and warm gently.

4. AZO DYE TEST:


To the compound in a test tube
add 2ml of concentrated
hydrochloric acid, cool. Take
sodium nitrite crystals in a Formation of orange-red Presence of amino group.
second test tube and dissolve it dye.
in concentrated hydrochloric
acid. In the third test tube take
β- naphthol and dissolve in
sodium hydroxide. Add the
contents of test tube 2 and 3 to
the organic compound.

RESULT:

The given sample contains ----------------------- functional group.

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