Activity No.

12
Qualitative Test for Elements in Organic Compounds

Group 4
Montes, Marie Therese Ann J.
Magan, Quinone
Mocorro, Maria Aiza L.
Obsioma, Jade A.
Perez, Jhonna lyn B.

BS Chemistry 2H1

Organic Chemistry Laboratory 1

Anorico, Nova Fe E.

November 25, 2021

 INTRODUCTION

1.1 Rationale

Carbon, hydrogen, sulphur, nitrogen, and halogen elements are some of the most
frequently occurring elements in organic compounds. Qualitative analysis can be used to
detect these elements, as there is no direct method for detecting oxygen.

Qualitative analysis is a technique used to determine changes in the melting

point, color, odor, radioactivity, reactivity, bubble generation, boiling point, and
precipitation of substances. On the other hand, quantitative analysis is a technique used to
determine the number of elements or molecules produced during a chemical reaction.
Thus, we can emphasize that qualitative analysis is a technique for identifying the species
contained within a compound and is more concerned with identifying the elements and
ions present, whereas quantitative analysis is concerned with determining the quantity
(how much) of elements contained within the compound.

Unknown organic compound identification and analysis is a critical aspect of

experimental organic chemistry. A systematic approach based on the scheme aids in
obtaining desirable results, as there is no one-size-fits-all set of procedures.

1.2 Objective of the Experiment

The aim of this experiment is to conduct a qualitative analysis in an organic

compound to determine the presence of elements nitrogen, sulfur, and halogens using
Lassaigne’s extract. The objectives are as follows:

1. To determine the presence of carbon, hydrogen, nitrogen, sulphur, and halogens in

organic compounds
2. To demonstrate the process of qualitative analysis of organic compounds
 MATERIALS AND METHODS

2.1 General Information

The materials that was used in the experiment are delivery tube with bulb, china dish, funnel,
tripod stand, wire gauze, distilled water, Bunsen burner, fusion tubes, test tubes, sodium
metal, small spatula, droppers, and forceps. The chemicals that was used are organic
compound, cupric oxide, anhydrous copper sulphate, lime water, freshly prepared sulphate
solution, ferric chloride solution, concentrated hydrochloride acid, Lassaigne's extract,
sodium nitroprusside solution, concentrated nitric acid, silver nitrate solution, ammonium
hydroxide solution, chlorine water, carbon disulphide, and dilute hydrochloric acid

2.2 Procedure

Detection of Carbon and Hydrogen

The organic compound was mixed with cupric oxide (CuO) three times its weight in a dry
test tube. The test tube was connected in a delivery tube with a bulb. The compound were
strongly heated. Observe the chemical reactions that occur in the process.

Detection of Nitrogen, Sulphur, and Halogens

Preparation of Lassaigne’s Extract

Small piece of sodium metal was taken by the used of forceps and were placed on a filter
paper. Then was dried by pressing it with another filter paper. Dried sodium was taken by the
used of forceps. The fusion tube were held by tongs and placed the dry sodium inside. The
fusion tube then was heated slightly over the Bunsen burner. A pinch of organic compound
was taken using the spatula and added into the fusion tube. The spatula was replaced. Fusion
tube is heated over the Bunsen burner again until becomes red hot. After heated, red hot tube
was plunge into the china dish that contains distilled water. Then the tube broke and crushed
with a glass rod. The process was repeated 2-3 times and heated the contents of the china dish
to boiling point for a few minutes. When the volume of the liquid in the china dish were
reduced to 1/3 or its initial volume, heating were stopped. Filter paper was taken and placed
in the funnel that is fixed to a stand. The contents of the china dish were filtered through the
funnel to a clean test tube that was placed under the funnel.

Detection of Nitrogen
Small amount of Lassaigne's extract was taken by the use of dropper and poured into a clean
test tube. Then, other dropper was used on getting the necessary amount sample of freshly
prepared ferrous sulphate solution and poured inside the test tube that contains Lassaigne's
extract. It was held by the test tube holder. The test tube is heated over the Bunsen burner.
After heating, test tube was placed in the test tube rack. Small amount of ferric chloride
solution was taken by another dropper and added into the contents of the test tube.
Concentrated hydrochloric acid was poured into the contents of the test tube by the used of
dropper.

Detection of Sulfur

Sodium Nitroprusside Test

Sodium Nitroprusside Test was the first for the detection of sulfur. Small amount of
Lassaigne's extract was taken by a dropper and poured into a clean test tube. Another dropper
was used to get a small amount sodium nitroprusside solution. Then, few drops of sodium
nitroprusside solution was added into the test tube that contains Lassaigne's extract.

Lead Acetate Test

The second is Lead Acetate Test. Small amount of Lassaigne's extract were taken by the used
of dropper and poured into a clean test tube. By the used of another dropper, small quantity of
acetic acid were taken and added into the test tube that contains Lassaigne's extract. Few
drops of lead acetate solution are also added into the contents of the test tube.

Detection of Halogens

Silver Nitrate Test

In Silver Nitrate Test, small amount of Lassaigne's extract are taken by the used of droppers
and was poured into a clean test tube. Other dropper was used on getting concentrated nitric
acid. Test tube holder were hsed to hold the test tube. Concentrated nitric acid then was added
into the Lassaigne's extract. The mixture inside the test tube were boiled over the bunsen
burner for some time. After, the contents of the test tube was cooled. Small amount of silver
nitrate solution was taken by another dropper and added inside together with the contents of
the test tube. Small amount of ammonium hydroxide is also collected by the used of dropper.
The test tube contains white precipitate of silver chloride was taken. Excess of ammonium
hydroxide is added into the test tube with silver chloride precipitate and were shaked well.
Ammonium hydroxide solution was taken by the dropper. Test tube contains the pale yellow
precipitate of silver bromide was taken. Ammonium hydroxide is added with silver bromide
precipitate and well shake the test tube that contains the mixtures. Again, ammonium
hydroxide was taken by dropper and added in silver iodide precipitate. The test tube that
contains the contents are shaken well.

Carbon Disulphide Test

In Carbon Disulphide Test, small amount of Lassaigne's extract were taken by the used of
dropper and poured in a clean test tube. Another dropper was used also to get small amount
of dilute hydrochloric acid. Then, dilute hydrochloric acid is added into the test tube that
contains Lassaigne's extract. Ample amount of carbon disulphide was taken by other dropper
and also added on the test tube. Chlorine water was taken by another dropper and poured into
the test tube that contains Lassaigne's extract then shake well.

The experimental setup of the conducted experiments are as follows:

Figure 2.1 Experimental setup of Detection of Carbon and Hydrogen

 Figure 2.2 Experimental Setup for Lassaigne’s Extract Preparation

Figure 2.3 Experimental Setup for Detection of Nitrogen, Sulphur, and Halogens
 RESULTS AND ANAYLSIS

This section discusses the results of the experiment.

Detection of Carbon and Hydrogen

As the evolved gas of organic compound and Cupric Oxide CuO passed through the bulb
with anhydrous copper sulfate CuSO4, the anhydrous copper sulfate turned blue indicating the
presence of hydrogen.

2 H+ CuO →Cu+ H 2 O

CuSO 4 +5 H 2 O →CuSO 4 ∙5 H 2 O

As the gas continues to pass through the delivery tube and into the lime water, the lime water
turned milky indicating presence of carbon in the compound.

C+ 2CuO → 2 Cu+CO 2

Ca(OH )2 +CO 2 →CaCO 3+ H 2 O

Detecting Nitrogen, Sulphur, and Halogens

Nitrogen, Sulphur, and halogens present in organic compounds are detected by Lassaigne’s
test. It is a general test for determining the presence of halogens, nitrogen, and sulphur in an
organic compound. Covalent bonds are formed between these elements and organic
compounds. These must be converted to their ionic forms in order to be detected. This is
accomplished through the fusion of the organic compound with sodium metal. The ionic
compounds formed during the fusion process are extracted and can be detected using simple
chemical tests. The sodium fusion extract is also known as Lassaigne's extract.

Test for Nitrogen

When the carbon and nitrogen in the organic compound combine with sodium metal, they
form sodium cyanide (NaCN), which is a water-soluble compound. By adding a sufficient
amount of ferrous sulphate, this is converted to sodium Ferrocyanide Na4[Fe(CN)6]. Ferric
ions generated during the process react with Ferro cyanide to form ferric Ferrocyanide
Fe4[Fe(CN)6] Prussian blue precipitate.

Na +C+ N → NaCN

6 NaCN + FeSO 4 → Na 4 [Fe (CN )¿¿ 6]+ Na2 SO 4 ¿

 3 +¿→ Fe4 [ Fe(CN )¿¿6 ]+12 NaCl¿ ¿
Na 4 [ Fe(CN )¿¿ 6]+ Fe ¿

The oxidation of ferrous ions is carried out by acids, which aid in the formation of ferric ions.
The presence of nitrogen in a solution can be confirmed by the presence of ferriferous
cyanide.

Test for Sulphur

Sodium nitroprusside is used to treat the extract. The violet color change indicates the
presence of sulphur.

2−¿+¿¿
S

Additionally, sulphur can be detected by adding lead acetate to SFE that has been acidified
with acetic acid. The presence of sulfur is indicated by the formation of a black precipitate
(PbS).

Pb ¿ ¿

Test for Halogens

Silver Nitrate Test

After acidification with HNO3, the extract is treated with AgNO 3. A white precipitate that is
slightly soluble in NH4OH indicates the presence of Cl, a yellowish precipitate that is slightly
soluble in NH4OH indicates the presence of Br, and a yellow precipitate that is completely
insoluble in NH4OH indicates the presence of I.
−¿¿

Cl−¿+ AgNO → AgCl +NO

3 3 ¿

AgCl+2 NH 3 OH →¿ ¿

The presence of bromine is confirmed by the formation of a pale yellow precipitate that is
partially soluble in NH4OH.
−¿¿
−¿+ AgNO3 → AgBr+ NO3 ¿
Br

Whereas the presence of iodine in the organic compound is confirmed by the formation of a
yellow precipitate that is insoluble in NH4OH.
−¿¿
−¿+ AgNO3 → AgI + NO 3 ¿
I
Carbon Disulphide Test

When sodium bromide and sodium iodide in Lassaigne's extract are treated with chlorine
water, the bromide and iodide oxidize to their halogen counterparts. This halogen reacts with
carbon disulphide to form carbon disulphide. Bromine colors the carbon disulphide layer
orange, while iodine colors it violet.

Cl 2+2 NaBr → Br 2 +2 NaCl

Cl 2+2 NaI → I 2 +2 NaCl

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