NAME : DZIA AMIRA YASMIN BINTI HELMY

MATRIC NO. : 23006227/1

OCC : 3

DEPARTMENT OF CHEMISTRY, FACULTY SCIENCE

UNIVERSITY MALAYA

ORGANIC CHEMISTRY 1 LAB REPORT

EXPERIMENT 3 : QUALITATIVE ELEMENTAL ANALYSIS

NAME OF LECTURER : DR-ING NURDIANA NORDIN

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Experimental Chemistry
EXPERIMENT 3 : QUALITATIVE
ELEMENTAL ANALYSIS
Dzia Amira Yasmin Binti Helmy
Faculty of Science, Department of Chemistry

University of Malaya
1/4/2023

Contents
Cover Page ..............................................................................................................................................1
1 Ovjective...............................................................................................................................................2
2 Introduction........................................................................................................................................2-3
3 Experimental Procedure.....................................................................................................................3-5
4 Results...............................................................................................................................................5-6
5 Discussions........................................................................................................................................6-8
6 Conclusions...........................................................................................................................................8
References..............................................................................................................................................8
Post-Lab Questions…………………………………………………………………………………8-9

1 Objective

To analyze and identify the elements present in benzamide through Lassaigne’s test, tests for

nitrogen, tests for sulphur, and tests for halogen.

2 Introduction

The analysis and identification of the structures of unknown substances constitutes a very

important part of experimental organic chemistry. Often, a common first step in the

identification of an unknown substance is to determine the elements present in the sample.

Organic chemists often use spectroscopic techniques to establish the structure of a compound.

However, it is often useful to supplement the spectral data with other information such as the

existence of elements other than carbon, hydrogen and oxygen. Elements such as nitrogen,

sulphur, iodine, chlorine, and bromine in organic compounds can easily be detected by means

of straightforward chemical tests.

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Nitrogen, sulphur, and halogens present in organic compounds are detected by Lassaigne’s

test. Here, a small piece of Na metal is heated in a fusion tube with the organic compound.

The principle is that, in doing so, Na converts all the elements present into ionic form.

Na (s) + C (s) + N (l) → NaCN (l)

2Na (s) + S (s) → Na2S (l)

Na (s) + X (l) → NaX (s) ( X= Cl, Br, or I)

The formed ionic salts are extracted from the fused mass by boiling it with distilled water.

This is called sodium fusion extract. [1]

A French chemist, J.L. Lassaigne has developed a method used for the qualitative

determination of elemental nitrogen, sulphur and the halogens in an organic compound

known as the Lassaigne’ test or more commonly as the sodium fusion test. [2] In this method,

the organic substance is heated with sodium metal under condition that ensure the conversion

of nitrogen, sulphur, and halides into ionizable inorganic substances as shown below:

3 Experimental Procedure

LASSAIGNE’S TEST

About 10 mg or one (1) (small) droplet of the unknown A (liquid) and about 50 mg of freshly

cut sodium metal were placed into a glass tube. The tube was heated with moderate heating to

avoid fast evaporation until the bottom of the tube is glowing red, the tube was holded at this

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heat for about 5 min. The hot tube was quickly plunged in an evaporating dish containing

distilled water (~ 10 mL) and cover the dish was covered quickly. The solution was boiled

on a hot plate for a few minutes while gently crushing the residue with a glass rod. Then, it

was filtered and a colourless filtrate has obtained.

TESTS FOR NITROGEN

About 0.5 mL of the filtrate was added to a tube containing about 0.2 g of powdered iron(II)

sulphate crystals. The mixture was heated gently while shaking until it boiled. Without

cooling, just sufficient dilute sulphuric acid was added to dissolve the gelatinous hydroxides

of iron. The solution formed was pale yellow in colour.

TESTS FOR SULPHUR

0.5 mL of the filtrate was acidified with dilute acetic acid. A few drops of 1% lead acetate

solution were added. Clear solution formed.

TESTS FOR HALOGENS

i. IF NITROGEN AND SULPHUR ARE ABSENT

A portion of the filtrate was acidified with dilute nitric acid and an excess of 5% silver nitrate

solution was added. White precipitate formed. Then, 2 mL 5% ammonium hydroxide was

added to the precipitate. The precipitate dissolved.

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iii. TESTS FOR IODINE

About 3 mL of the filtrate was acidified with 10% sulphuric acid solution and it was heated

until it was boiling for a few minutes. After cooling, 1 mL of dichloromethane was added

followed by a drop of 5% sodium hypochlorite (bleach). Colourless solution formed.

iv. TESTS FOR BROMINE

About 3 mL of the filtrate was acidified with 10% sulphuric acid solution and it was heated

until it was boiling for a few minutes. After cooling, 1 mL of dichloromethane was added

followed by a drop of 5% sodium hypochlorite (bleach), while shaking, until a possible

purple colour (presence of iodine) has disappeared. Colourless solution formed.

v. OTHER TESTS FOR HALOGENS

To test for chlorine in the presence of iodine and/ or bromine, the filtrate was acidified with

5% nitric acid and the solution was boiled for a few minutes. Enough 0.1 M silver nitrate was

added to precipitate out the halogen completely as silver halides. The precipitate was filtered

and about 3 mL of 0.1% NaOH (aq) solution was added. The mixture was boiled for about 2

minutes and the solution was filtered. The filtrate was acidified with 5% nitric acid and a few

drops of 0.1 M silver nitrate (aq) were added. No white precipitate formed.

4 Results

Results :
Unknown : Benzamide
Colour : White
Physical appearance : White solid
Other characteristics : Insoluble on water and more soluble in aqueous ammonia.

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Test Observation Inference
Nitrogen Pale yellow solution formed. Nitrogen is absent in this
compound.

Sulphur No black precipitate formed. Sulphur is absent in this

compound.

Halogens (absence White precipitate formed. Chlorine is absent in this

of N & S) compound. (White precipitate
indicates silver chloride)
Iodine No purple or violet colour Iodine is absent in this
appeared. compound.

Bromine No reddish-brown colour Bromine is absent in this

appeared. compound.

Other tests for No white precipitate formed. Chlorine is absent in this

halogens compound.

Table 1 : Observation and inference of each tests results.

5 Discussions

Based on Table 1, As we know, benzamide is a compound that consists of three type of

elements which are hydrogen, carbon, and a heteroatom nitrogen. In this experiment,
Lassaigne’s test, tests for nitrogen, tests for sulphur, and tests for halogens are carried out to
confirm that the only heteroatom present in this compound is nitrogen. Based on Lassaigne’s
test, colourless filtrate is obtained. It means that sodium cyanide (NaCN)(s) is formed from
the reaction between sodium metal and benzamide. The sodium metal is used to convert all
the elements (nitrogen, sulphur, and halogen) in the compound into ionic form. The chemical
equation involved is C (s) + N (l) + Na0(s) → NaCN(s). The products formed when sodium
metal is added to an unknown compound are depend on the elements present in a compound.
We can’t determine which products are formed from the Lassaigne’s test, whether NaCN(s),
Na2S(s), or NaX(l) if the compound is an unknown and we can’t identify what elements are
present in that unknown compound. Therefore, we have to carry out the other tests which are

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tests for nitrogen, tests for sulphur, and tests for halogens to test specifically which elements
are present in the unknown compound.

Based on the tests for nitrogen, a negative result which is pale yellow solution is formed. The
formation of pale yellow solution means that the nitrogen is absent. So, from this test, we can
confirm that nitrogen is not present in benzamide.

Based on the tests for sulphur, no black precipitate is formed when the lead acetate is added
to the filtrate and this is a negative result. This negative result can let us confirm that
benzamide does not consist of sulphur element. It means the lead sulphide that gives black
precipitate does not form due to no sulphide ion is absent in benzamide.

From the tests for halogens (if nitrogen and sulphur are absent), a positive result is obtained
which white precipitate is formed when aqueous silver nitrate is added to the fusion solution.
The white precipitate indicates the presence of chlorine. When the silver nitrate is added,
silver chloride was formed. This make us confirm that the chlorine halogen is present in
benzamide.

Based on the tests for iodine, the result obtained is negative which means no production of
purple or violet in the dichloromethane layer. When the dichloromethane is added, no iodide
ion reacted with the dichloromethane. Therefore, purple or violet precipitate of iodide ion did
not appear. The negative result from this test is a conformation of the absence of iodine in
benzamide.

Based on the tests for bromine, no reddish-brown colour solution is formed. It means that no
reaction occurred between the bromine ion and dichloromethane due to the absence of
bromine in this compound. The negative result of the tests for bromine confirmed that
bromine is absent in the benzamide.

Based on the other tests for halogens, a negative result is obtained and no white precipitate is
formed. The purpose of this test is to test the presence of chlorine in the presence of iodine
and/or bromine. After the silver nitrate is added to the filtrate, no white precipitate is formed

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meaning that doesn’t have chloride ion to react with the nitrate ion from the silver nitrate to
form silver chloride. This result shown that chlorine is absent in benzamide.

6 Conclusion
The only heteroatom presents in benzamide is chlorine while the others (nitrogen, bromine,

and iodine) are absent in benzamide.

References

1. (2023, August 29). Lassaigne’s Test - Test for Nitrogen, Sulphur, Halogens with
Examples.

BYJUS. https://byjus.com/jee/lassaigne-test/

2. CALHOON JR, S. W. (1963). A SIMULTANEOUS DETERMINATION OF CARBON,

HYDROGEN, AND NITROGEN IN SOME NITROGENOUS ORGANIC COMPOUNDS.
The Ohio State University.

Post-lab Answers:

1) Write the reaction equation for the formation of a black precipitate if sulphur is

present in the sample.

Pb2+ (aq) + S2− (aq) → PbS (s)

2) The mixture is boiled in a fume cupboard to expel nitrogen and sulphur that may

be present in the sample. Explain.

Nitrogen and sulphur are poisonous elements that may harm human health. Furthermore,

when the mixture is boiled, cyanide gas and sulphide gas will be released. Both cyanide gas

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and sulphide gas are poisonous gas. Cyanide gas is explosive gas that may cause an explosion

at a high concentration. Moreover, if humans breathe in too much poisonous or toxic gas,

cellular respiration will be interrupted. Therefore, to repel nitrogen and sulphur by boiling the

mixture must be carried out in a fume cupboard to ensure our safety.

3) How are the sodium wastes in the experiment destroyed?

Sodium is a very reactive element so it must be destroyed in a waste bottle specialized for

disposal of sodium. Sodium wastes can be put in a bottle and labelled as sodium hydroxide in

water-ethanol for disposal because sodium wastes can be destroyed readily in 95% ethanol.

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