Organic and Inorganic Analysis 1

Course 126: Exp No-04

Name of the experiment:

Detection of Elements: Lassaigne's Test

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 Objectives 2

This experiment is designed for this course to make the student capable-
Course 126: Exp No-04

➢The objective of this experiment is to detect the presence of nitrogen, sulphur, and

halogen (chlorine, bromine and iodine) in organic compounds by Lassaigne's test.

➢ To use reagent grade chemicals to identify elements in organic compounds.

➢ To use simple apparatus to identify elements in organic samples.
➢ To understand the reaction and its mechanism.
➢ To observe change of colour for different reactions related with to this analysis.

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 Theory 3

➢In this experiment, organic compounds are fused with metallic sodium to convert the
Course 126: Exp No-04

elements (N, S, X) into water soluble sodium salt. As we know, organic compounds are non-polar
and insoluble in water so, to make it polar and to form soluble ion, sodium fusion method is
used. Then prepared ionic solution (ions) react with respective reagents to detect elements such
as nitrogen, sulphur and halogens.

➢There are several ways to detect element in organic compounds such as spectroscopic
analysis, elemental analysis etc. But these techniques are expensive and time consuming. On the
other hand, by using Lassaigne test we can identify nitrogen, sulphur and halogens present in
organic compounds easily. This is inexpensive and can detect element within a short time.

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 Detection of Nitrogen 4
Course 126: Exp No-04

Detection of Nitrogen:
If nitrogen is present in the compound, the Lassaigne's extract would contain sodium cyanide
formed during fusion. Sodium cyanide is converted to sodium ferrocyanide on treating with
ferrous sulphate. On further treating it with ferric chloride, a prussian blue complex,
ferricferrocyanide is formed.

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 Reactions 5

Reactions for detection of nitrogen

Course 126: Exp No-04

Fuse
Na + C + N NaCN
(From organic compound)
FeSO4 + 2 NaOH Fe(OH)2 + Na2SO4
Green ppt
Fe(OH)2 + 2 NaCN Fe(CN)2 + 2NaOH
(From Sodium extract)
Prussian Blue Colour

Fe(CN)2 + 4NaCN Na4[Fe(CN)6]

Sodium ferrocyanide

3Na4[Fe(CN)6] + 4FeCl3 Fe4[Fe(CN)6]3 + 12 NaCl

Ferric ferocyanide
(Prussian blue/green) Prussian Blue PPT
and Green PPT
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 Detection of Sulphur 6
Course 126: Exp No-04

Detection of Sulphur
1. Sodium nitroprusside test
During the preparation of Lassaigne's extract, sulphur from the organic compound reacts
with sodium to form sodium sulphide. It gives a purple colour with sodium nitroprusside
due to the formation of sodium thionitroprusside.

Sodium thionitroprusside (Violet Colour)

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 Test of Sulphur 7
Course 126: Exp No-04

2. Lead acetate test

Sodium sulphide formed during the preparation of Lassaigne's
extract reacts with lead acetate to yield lead sulphide as black
precipitate.

Black ppt of Lead Sulphide

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 Test of Chlorine 8

Chlorine:
Course 126: Exp No-04

During the preparation of Lassaigne's extract, chlorine form the organic compound reacts with
sodium to form sodium chloride. Sodium chloride gives a white precipitate of silver chloride with
silver nitrate solution. The precipitate is soluble in ammonium hydroxide.

White ppt of Silver Chloride

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 Test of Bromine 9
Course 222: Exp No-04

b. Bromine
Sodium bromide formed during the preparation of Lassaigne's
extract reacts with silver nitrate to form pale yellow precipitate
of silver bromide, which is sparingly soluble in ammonium
hydroxide.

Pale yellow ppt of Silver Bromide

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 Test of Iodine 10
Course 222: Exp No-04

c. Iodine
Sodium iodide formed during the preparation of sodium fusion
extract reacts with silver nitrate solution to form yellow
precipitate of silver iodide, which is insoluble in ammonium
hydroxide.

Yellow ppt of Silver Iodide

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 Preparation of stock solution 11

Procedure:
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➢ At first, take a small oil free sodium metal in a dry fusion tube.
➢ Add very little amount of supplied organic sample to the sodium metal into the fusion tube.
➢ Then burn this fusion tube with sodium and sample properly up to make it red color.
➢After burning properly, put it in a mortal with small amount of water and make it powder (in
solution) with pestle.
➢ Then filter this solution by using a filter paper.
➢ Keep this filtrate as stock solution.
This stock solution will be used for detecting nitrogen, sulfur and halogen.
fuse
Organic compounds containing N,S,X + Na (metal) NaCN/ Na2S/ NaSCN/ NaX

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 Preparation of stock solution 12
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Experiment :
(Video)

Sodium metal under

liquid paraffin
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 Test of Nitrogen 13

a. Test for nitrogen (N):

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➢ Take 1 or 2 mL of stock solution in a test tube

➢ Add 2-3 drops of freshly prepared saturated solution of FeSO4 or directly you can add solid
FeSO4.
➢ Boil the mixture for about 1 minute and 2-3 drops of FeCl3 solution.
➢ Add dilute HCl to render the solution acidic until any precipitate forms.

6 NaCN + FeSO4 Na4[Fe(CN)6] + Na2SO4

3Na4[Fe(CN)6] + 4FeCl3 Fe4[Fe(CN)6]3 + 12 NaCl

Ferric ferocyanide
(Prussian blue/green)

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 Test of Nitrogen 14
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Observation: Prussian blue precipitate or green colour solution was observed.

Inference: Positive (Nitrogen present). If no blue ppt or green solution was found, Negative
(Nitrogen absent)

Positive Positive

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 Test of Sulphur 15

b) Test for sulphur (S):

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i) Lead acetate test:

Procedure:
➢ Acidify a portion of the stock solution by adding acetic acid dropwise
➢ Add 2-3 drops of saturated lead acetate solution.

Na2S + Pb(CH3COO)2 PbS + 2CH3COONa

Black ppt

Observation: Black precipitate was observed.

Inference: Positive (sulphur present).
Black ppt of PbS

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 Test of Sulphur 16

ii) Sodium nitropruside test:

Course 222: Exp No-04

Procedure:
➢Take 1-2 mL of the stock solution
➢ Add 2-3 drops of freshly prepared sodium nitropruside solution.

Na2S + Na2[Fe(CN)5NO] Na4[Fe(CN)5NOS]

Sodium nitroprusside Sodium thionitroprusside
Violet colour

ii) Observation: Violet ppt was found,

Inference: Sulphur present
Violet colour of sodium nitropruside
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 Combined Test of Sulphur and Nitrogen 17

c) Combined test of N and S :

Course 222: Exp No-04

Procedure:
➢ Take 1 or 2 mL of stock solution in a test tube and boil the solution for about 1 minute
➢ Add 2-3 drops of FeCl3 solution.

NaSCN + Fe3+ [Fe(SCN)]2+

Reddish brown/Red ppt

Reddish brown/Red
Observation: Reddish brown/Red precipitate was observed.
precipitate of ferric
Inference: Positive (Nitrogen & sulphur present). thiocyanate

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 Test of Halogen 18
Course 222: Exp No-04

c) Test for halogen (Cl, Br, I):

i. Silver nitrate test:

➢ Acidify a portion of the stock solution with dilute nitric acid, boil until it has been reduced to
half of its original volume.
➢ Cool and add 1% silver nitrate (AgNO3) solution.
➢ A heavy white precipitate indicates the presence of chloride, pale yellow indicates presence
bromide and yellow indicates presence of iodide in the supplied sample.

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 Experiment 19

NaCl + AgNO3 AgCl + NaNO3

Course 222: Exp No-04

White ppt

NaBr + AgNO3 AgBr + NaNO3

Pale yellow ppt

NaI + AgNO3 AgI + NaNO3

Yellow ppt

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 Test of Halogen 20

ii) Further confirmation by ammonia solution:

Course 222: Exp No-04

After forming precipitate, add dilute ammonia solution to the precipitate (ppt). If the ppt is
white and readily soluble in ammonia solution, chloride is present. If it is pale yellow and
sparingly soluble in conc. ammonia solution, bromide is present. If it is yellow and insoluble in
ammonia solution the iodide is present.

AgCl + 2NH4OH [Ag(NH3)2]Cl + 2H2O

Soluble

AgBr = Sparingly soluble in NH4OH

AgI = Insoluble in NH4OH

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 Result for unknown sample 21

Results
Course 222: Exp No-04

Observation:
Sample A: A-----colour ppt was formed
Sample B: A-----colour ppt was formed
Sample B: A-----colour ppt was formed

Inference:
1. Sample A might be contain-
2. Sample B might be contain-
3. Sample C might be contain-

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