Paper: Lab – 50

Syllabus
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Experiment: Organic Qualitative analysis
1) Detection of elements (Nitrogen, Sulphur and halogens).
2) Detection of functional groups of organic compounds by qualitative method.
3) Practical Note Book
4) Viva
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(Writing model for laboratory note book)

Experiment No. 1: To identify the presence of elements and functional group present in
the given organic sample.
1. Preliminary test of organic sample:
Experiment Observation Inference
i) Colour and physical state Reddish brown liquid Compound may
substance. contain amine group.
ii) Odour Aniline like smell. Aromatic amine may
be.
i) Solubility Insoluble in water but Amine may be.
soluble in dilute acids.

ii) Litmus test: Red litmus turned blue. Amine may be.

iii)Flame test: Placed the compound Smoky flame. Aromatic compound.

(about 0.1 g) on a nickel spatula and
heated over a burner flame.

iv) Unsaturation test:

a) 1 mL of organic substance or its Precipitate appear but no Saturated compound.
 solution + bromine water. change colour of bromine
solution.
b) 1 mL of organic substance or its No decolourisation of Saturated compound.
solution + 1 mL dil. H2SO4 + 2 KMnO4 solution.
mL alkaline KMnO4 solution.

2. Detection of elements present (Procedure for Lassaigne’s test): Taken a small piece of
(0.04 g) freshly cut sodium metal and dried by pressing in between a filter paper. Taken a dry
and clean fusion tube and placed inside the small piece of sodium metal. Heated the fusion
tube until formation of sodium vapour (dark grey in colour) and poured the small amount of
powdered organic sample portion directly on to the molten sodium. Heated the fusion tube to
redness for about two minutes and carefully dipped the hot tube along with fusion residue in a
porcelain basin having distilled cold water and crushed the tube. Boiled the resulting product
and filtered the hot solution and washed the residue with distilled water. From the
Lassaigne’s filtrate the following tests are preformed.

Experiment Observation Inference

1. Taken 2-3 mL of Lassaigne’s filtrate in a A Prussian blue Nitrogen is present.
test tube and add 0.1-0.2 g of powdered precipitate is obtained.
iron(II) sulphate. Heated the mixture and
at hot condition added dilute sulphuric
acid to dissolve the iron hydroxide.

2. (a) Added few drops of dilute acetic acid No precipitate is Sulphur is absent.
to 2-3 mL of Lassaigne’s filtrate and obtained.
added few drops of lead acetate solution.

(b) Added 2-3 drops of freshly prepared No purple coloured Sulphur is absent.
dilute solution of di-sodium solution.
pentacyanonitrosyl ferrate (sodium
nitroprusside) to 2-3 mL of Lassaigne’s
filtrate.

3. Added few drops of dilute nitric acid to (a) No precipitated. Chlorine is absent.
2-3 mL of Lassaigne’s filtrate and added
excess amount of sliver nitrate solution.
(b) No precipitated. Bromine is absent.

(c) No precipitated. Iodine is absent.

3. Tests for functional group present in given organic substance:

Experiment Observation Inference

1. Test for alcoholic hydroxyl group:
Ester test: 0.1 g of organic substance + 1 No ester smell Alcoholic hydroxyl
mL of conc. H2SO4 + 1 mL glacial acetic appeared. (-OH) group is
acid. Heated the mixture for five minutes. absent.

2. Test for phenolic hydroxyl group:

Liebermann’s test: Organic substance + 2-
3 crystals of sodium nitrite then heated. On
cooling-
a) Added 1 mL conc. H2SO4 No coloured Phenolic (-OH)
precipitate appeared. group is absent.

ii) Poured the above mixture in a beaker No change of colour Phenolic (-OH)
containing water of the solution. group is absent.

iii) Made the above mixture alkaline by No change of colour Phenolic (-OH)
adding NaOH solution. of the solution. group is absent.

3. Test for carbonyl group:

a) Sodium bisulphite test: 2-3 crystals No precipitate Carbonyl (-CHO or
of organic substance + 2 mL sodium appeared. >C=O) group is
absent.
bisulphite solution. Allowed the
mixture undisturbed.
b) 2,4-Dinitrophenyl hydrazine No yellow or
red Carbonyl (-CHO or
(Brady’s reagent) test: 1 mL precipitate appeared. >C=O) group is
absent.
alcoholic solution of organic
substance + solution of 2,4-
dinitrophenyl hydrazine. Kept the
solution in hot water for 15 minutes
 and then allowed cooling.

4. Test for carboxyl group:

a) Sodium bicarbonate test: 1 mL No evolution of gas. Carboxyl(-COOH)
aqueous solution organic substance + group is absent.

solid NaHCO3.
b) Ferric chloride test: 1 mL aqueous No change of the Carboxyl (-COOH)
solution organic substance + neutral colour of the solution. and phenolic
solution of ferric chloride. hydroxyl group is
absent.

5. Test for amine group:

a) Azo dye test: Dissolved the organic Bright coloured dye Amine (-NH2) group
substance in 1-2 mL dil. HCl and appeared. is confirmed.
cool the solution by ice water. In
cold condition added concentrated
solution of NaNO3. Again in cold
condition added few drops of
alkaline solution of β-naphthol.
b) Carbylamine test: Organic Offensive smelling Primary amine (-
substance + 2 mL alcoholic KOH gas evolved. NH2) group is
solution + 2-3 drops of chloroform. confirmed.
Heated the mixture.

6. Test for amide group:

a) Test with nitrous acid: Taken 0.5 g No effervescences are Primary aliphatic
of organic substance in alcohol and detected. amide group is
added few volume of nitrous acid absent.

b) Test with alkali: Taken 0.5 g of No smell of ammonia. Primary aliphatic

organic substance and added excess amide group is
amount of concentrated sodium absent.
hydroxide solution and boiled the
content.
 c) Test with hydroxylamine No bluish red coloured Aromatic amide
hydrochloride: Taken 0.5 g of solution. group is absent.
organic substance and added few
amount of alcoholic solution of
hydroxylamine hydrochloride.
Boiled the content for five minutes
and allowed cooling. In cold
condition added 4-5 drops of dilute
ferric chloride solution.

d) Biuret test: Heated 0.5 g of organic No pink colour Compound is not

substance in a test tube for developed. urea.
elimination of vapour (if evolve) and
added 1 mL of dilute alkali on cold
condition and then added two drops
of dilute copper sulphate solution.
7. Test for hydrocarbon:
a) Iodine test: 0.2 g of organic Violet colour is not Hydrocarbon is
substance (2-3 drops if it is liquid) + persistent. absent.
5 mL benzene in a test tube. Above
solution + 5 mL of very dilute
solution of iodine (in benzene)
b) Friedel-Crafts test: Heated 0.1 g of No dye is produced. Aromatic
AlCl3 in a dry test tube + 2-3 drops hydrocarbon is
of mixture of equal amounts of absent.
organic substance and chloroform to
AlCl3.

Conclusion: From the above systematic experiments it is found that the given organic
substance contain nitrogen as element and it contains primary amine (-NH2) group.
N.B: Mention the reactions for positive tests in the left hand side of the laboratory note book
only by pencil.
(Don’t write in laboratory note book)
Precautions
a) Do not try to inhale organic compounds as most of organic compounds are
poisonous.
b) Chloroform should use in the presence of laboratory attendants.
c) Do not try to inhale the gas evolved in carbylamine test.
d) Always use the minimum amount of available reagent. Do not mention the test which
is not done practically in the laboratory.
e) Mention two positive tests for a functional group and one negative for each functional
group.

Materials collected and prepared from:

J. Borah etal, Practical Chemistry, Kalyni Publishers
Jyotishmoy Borah