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PART-B: Analysis of organic Compounds

Detection of Elements (Qualitative Analysis)


a) Detection of Carbon and Hydrogen

b) Detection of Nitrogen

c) Detection of Nitrogen and Sulphur present together

d) Detection of Sulphur

e) Detection of Halogen (Chlorine, Bromine and Iodine)

Mrs Vinita Nema


Detection of Carbon and Hydrogen

• Carbon must be present in a compound Glass wool


under examination if it is definitely known
to be an organic compound. Similarly,
hydrogen too, is generally present. Both
these elements can be tested together.
• A small quantity of the dry and powdered
substance is mixed with freshly ignited
cupric oxide.
• The mixture is heated in a well-dried hard
glass test-tube provided with a delivery
tube having a bulb at one end.
• The other end of the tube is dipping under
lime water taken in another test tube.
• Carbon present in the compounds is
oxidised to carbon dioxide which turns lime
water milky

Mrs Vinita Nema


Detection of Carbon and Hydrogen

The hydrogen present in the compound is

oxidised to water which condenses on the

cooler parts of the test tube or in the bulb of

delivery tube. The drops turn white anhydrous

copper sulphate placed in the bulb into blue.

Mrs Vinita Nema


Detection of Nitrogen

Lassaigne’s Test
This test is a confirmatory test for nitrogen in
organic compounds. This test involves two steps:

(a) Preparation of Lassaigne’s extract.

A small piece of a sodium metal is heated gently in


a fusion tube till it melts to a shining globule. At
this stage, a small amount of substance is added
and the tube is heated strongly.
The red hot tube is plunged into distilled water
contained in a china dish. The contents are boiled
for some time, cooled and then filtered. The
filtrate is known as sodium extract or Lassaigne ‘s
extract. • The purpose of fusing the organic compound with Na metal
before the detection of elements to convert the co-valent
organic compounds in to ionic compounds.
Mrs Vinita Nema
Detection of Nitrogen
b) Procedure of the test
i) One part of S.E. is made alkaline by adding of
few drops of NaOH.
ii) Alkaline S.E. is boiled with freshly prepared
Ferrous sulphate solution.
iii) Cool the solution and then acidify with dil
H2SO4 (to avoid the yellow colour of ferric
chloride) and then add FeCl3.
c) Observations
A Prussian Blue or Green Colour

• The purpose of acidifying the reaction mixture in


the end is to dissolve any green ppt. of
Fe(OH)2 since it may lead to wrong inferences.
• When the alkaline solution is acidified with HCl
the yellow colour of FeCl3 makes the blue colour • On fusion with Na metal hydrazine does not form NaCl due
to the absence of carbon.
to appear green.
• Dizonium salts are unstable on heating they nitrogen and
• Li and K can not be used in place of K because Li will not give positive test for nitrogen
reacts slowly whereas K reacts vigorously. Mrs Vinita Nema
Detection of Nitrogen and sulphur present together

If the organic compound contains both nitrogen and sulphur, sodium sulphocyanide (NaCNS) is formed
during preparation of Lassaigne’s extract. Sodium sulphocyanide reacts with ferric chloride and gives
blood red colouration due to formation of ferric sulphocyanide

Thus, appearance of a blood red colouration on performing Lassaigne’s test for nitrogen indicates the
presence of both nitrogen and sulphur in the organic compound
Mrs Vinita Nema
Questions….?

1. What is the purpose of organic fusing the organic compound with sodium metal before testing for N, S
or helogen?
2. Why Li and K can not be used in place of sodium in Lassaigne’s Test for elements?
3. Why the Lassaigne’s Test for nitrogen is not showing by dizonium salts and hydrazine?
4. During the Lassaigne’s Test for nitrogen with S.E. sometime a blood red colour obtained with FeCl3
why?
5. Why do we add suphuric acid during the Lassaigne’s Test for nitrogen?
6. What happens when we add dil HCl instead of dil H2SO4 during the Lassaigne’s Test for nitrogen?

Mrs Vinita Nema


Detection of Sulphur

1. Sodium nitroprusside test. To a small portion of Lassaigne’s extract add a few drops of sodium
nitroprusside solution. A purple colouration of sodium pentacyanonitrosyl suplfide
ferrate (III) indicates the presence of sulphur in the compound.

Chemistry of the test


During preparation of Lassaigne’s extract sulphur from the organic compound combines with sodium to
form sodium sulphide. Sulphides give purple colouration on reaction with sodium nitroprusside.

Mrs Vinita Nema


Detection of Sulphur

2. Lead acetate test. Acidify a small portion of Lassaigne’s extract with acetic acid and add a few
drops of lead acetate solution. The formation of black ppt. of Lead sulfide indicates the presence of
sulphur in the compound.

• Suplphuric acid is not used for acidification of because it will form white precipitate of lead sulphate with
lead acetate which will interfere with the test.
• Acidic acid is used before adding the lead acetate because the black precipitate of lead sulfide is
insoluble in acidic medium.

Mrs Vinita Nema


Questions….?

1. Sulphuric acid is not used for acidification of sodium extract during the Lassaigne’s Test for Sulphur.
2. Why is sodium extract is made acidic before the addition of lead acetate in the detection of suplhur
by Lassaigne’s Test?

Mrs Vinita Nema


Detection of Halogen (Chlorine, Bromine and Iodine)

Silver nitrate test. To a small portion about 2 ml of


Lassaigne’s extract add 1 ml of cone, nitric acid and boil for
some time. Cool the contents and add to it silver nitrate
solution.
(a) White precipitate, soluble in ammonium hydroxide,
indicates the presence of chlorine in the organic compound.
(b) Pale yellow precipitate, sparingly soluble in
ammonium hydroxide, indicates the presence of bromine in
the compound.
(c) Yellow precipitate, insoluble in ammonium hydroxide,
indicates the presence of iodine in the organic compound.

Mrs Vinita Nema


Detection of Halogen (Chlorine, Bromine and Iodine): Chemistry of the test

(c) For Iodine


(a) For Chlorine

The function of adding cone. HNO3 and boiling is to


decompose any sodium cyanide or sodium sulphide
(b) For Bromine present in the extract. Otherwise these compounds
will interfere with the tests of halides since NaCN
gives a white ppt. with silver nitrate while Na2S gives
a black ppt.

Mrs Vinita Nema


Questions….?

1. Why it is necessary to boil the sodium extract with Conc HNO3 before testing for halogens?

Mrs Vinita Nema

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