Qualitative Tests for Elements in Organic Compounds

Exercise 5

Rovic Kevin N. Mellado

Emma Buncales

CHY 42.1

TTH 7-10 AM
 Introduction

Qualitative analysis is always applied as a first step in identifying a compound when a new
compound is readily prepared or isolated from some natural source. In an organic compound,
elements carbon, hydrogen and oxygen are assumed to be present commonly. Nitrogen, Sulphur
and halogens (chlorine, bromine and iodine) may also present in the organic compound. The
identification of elements in a given compound is a type of qualitative analysis since the
experiment is dealing with the composition of a unknown compound. This experiment must be
handled very carefully as further the analysis of the organic compound is according to the element
present in it. Generally, the traditional technique is only can be applied to inorganic ions in aqueous
solution. This experiment was conducted with the following objectives: To identify the different
kind of test for elements in organic compounds; To carry out the different tests in order to
determine the elements present in the test solutions; To identify the elements present in compounds
and their coloration.
 Methodology

A. Materials and Apparatus

The Chemicals used in the experiments are as follows: Ferrous Sulfate, Ferric
Chloride, Sulfuric Acid, Soda Lime, Acetic Acid, Nitric Acid, Sodium
Nitroprusside, Lead acetate, Silver Nitrate, Hydrochloric Acid, Benzene and Ethyl
Alcohol.

The Apparatus used include Alcohol Lamp, Wire gauze, Iron Stand, Iron ring,
Beaker, Test tube Holder, Test tube Rack, Stirring rod, Litmus Paper, Ferrox Paper.

B. Procedure

1. Test for Nitrogen

a. Lassaigne’s Test
- Two drops of saturated Ferrous Sulfate solution were added to 2mL of the test
solution. Enough 40% NaOH was added to produce alkalinity. It was then
boiled and filtered to remove FeS. 5M sulfuric acid and two drops of ferric
chloride solution was then added to acidify the filtrate. A precipitate of Prussian
Blue indicates the presence of nitrogen.

b. Soda Lime Test

- A pinch of test compound with a small amount of soda lime was heated in a dry
test tube. A small piece of moist litmus paper was exposed on the end of the
stirring rod when the vapors were formed. The color changes when it encounters
the vapor. The other end of the stirring rod was then dipped in concentrated HCl
and exposed to the vapors evolved.
2. Test for sulfur
a. Lead sulfide test
- 2mL of test solution was acidified with dilute acetic acid. A few drops of lead
acetate solution were then added.
b. Sodium Nitroprusside test
- 2 drops of sodium nitroprusside solution were added to 2mL test solution. A
deep reddish violet solution indicates the presence of sulfur.

3. Test for Halogens

- 2mL of test solution was acidified with dilute nitric acid. 3 drops of silver nitrate
solution were added and boiled for 3 minutes. The formation of precipitate
which is insoluble in hot nitric acid indicates the presence of halogens. A white
precipitate contains chlorine, light yellow contains bromine and dark yellow
contains iodine.

4. Test for Oxygen

- Ferrox paper were placed separately into three dry test tubes. 10 drops of
benzene were added to the first test tube. 10 drops of ethyl alcohol were added
to the second test tube and 10 drops of test liquid were added to the third test
tube.
 Results

Table 1. Observations of Organic Compounds on Nitrogen Test

Test Observations Inference

Lassaigne’s Test 1. Some dark green Nitrogen is Present
precipitate and a little amount
of dark precipitate were
formed after brownish orange
FeSO4 is added.
2. The precipitate become
greenish after more FeSO4 is
added.
3. The color of precipitate
remained unchanged after
heating.
4. The precipitate did not
change after Sulfuric acid is
added.
5. Blue precipitate is formed
immediately after adding of
FeCl
Soda Lime Test 1.urea decomposes and the Nitrogen is Present
nitrogen in the form of amino
nitrogen liberated ammonia
gas.
2. formation of Prussian blue
after the sodium fusion.
3. Red litmus paper changes
to blue
 Table 2. Observations of Organic Compounds on Sulfur Test

Observation Inference
Lead Sulfide test A black precipitate is formed. Sulfur is Present

Sodium nitroprusside test A deep purple solution is Sulfur is Present

formed immediately.

Table 3. Observations of Organic Compounds on Halogens

Observation Inference
Test Tube A Formation of white Halogen is Present (Chlorine)
precipitate after nitric acid
and silver nitrate are added.
Test Tube B Formation of yellow Halogen is Present (Bromine)
precipitate after nitric acid
and silver nitrate are added.
Test Tube C Formation of dark yellow Halogen is Present (Iodine)
precipitate after nitric acid
and silver nitrate are added.

Table 3. Observations of Organic Compounds on Oxygen Test

Observation Inference
Toluene Transparent No Presence of Oxygen
Ethanol Deep Red Precipitate Presence of Oxygen
Water Deep Red Precipitate Presence of Oxygen
 Discussion

In Lassaigne’s test, the carbon and nitrogen that are present in the organic compound on fusion
with sodium metal gives sodium cyanide. This is converted into sodium ferrocyanide by the
addition of enough quantity of ferrous sulphate. Ferric ions generated during the process react with
ferrocyanide to form Prussian blue precipitate of ferric ferrocyanide.

2NaCN + FeSO4→Fe (CN)2 + Na2SO4

Fe (CN)2 + 4NaCN → Na4[Fe (CN)6]

Sodium ferrocyanide

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

Ferric ferrocyanide

In Soda Lime Test, the results show that Nitrogen is usually detected by the formation of
Prussian blue after the sodium fusion as it turns the red litmus paper to blue.

In the Lead Sulfide test, the results show that when sulfur containing amino acids like cysteine
is heated with strong alkali like NaOH, some of the sulfur is converted to sodium sulfide (Na2S)
which can be detected by precipitation as lead sulfide (PbS) from alkaline solution.

Na2S + Pb (CH3COO)2 → PbS

Lead acetate Black precipitate

In Sodium nitroprusside Test, the results show that If Sulfur is present in the organic
compound, sodium fusion will convert it into sodium sulfide. Sulfide ions are readily identified
using sodium nitroprusside.

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

Sodium nitroprusside violet color

 In the test for Halogens, the results showed that the sodium fusion extract is acidified with
nitric acid and then treated with silver nitrate.

Na + X → NaX

NaX + AgNO3 → AgX (X − Cl, Br, I)

A white precipitate soluble in ammonium hydroxide (NH4OH) shows the presence of chlorine.

Cl− + AgNO3 → AgCl ↓ (white ppt) + NO3−

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

A light yellowish precipitate sparingly soluble in NH4OH shows the presence of bromine.

Br− + AgNO3 → AgBr ↓ (light yellow ppt) + NO3−

A dark yellow precipitate insoluble in NH4OH shows the presence of iodine.

I− + AgNO3 → AgI ↓ (dark yellow ppt) + NO3−

In the Oxygen test, the results showed that the presence of oxygen may be determined either
with the use of ferrox paper. In the presence of oxygen containing compounds, the complex
FeCNS++ gives a deep red colored solution as it distributed between the filter paper and the test
compound.
 Summary and Conclusion

In this experiment, six different tests were done to identify the compounds and the structures
for elements in organic compounds. Nitrogen was identified through the Lassaigne and the Soda
Lime tests, in which both experiments indicated a blue precipitate around the test tube indicating
the presence of nitrogen. Sulfur was identified through the Lead Sulfide and the Sodium
nitroprusside test in which a black and purple precipitate were formed, indicating the presence of
Sulfur. The presence of Halogens was also identified using silver nitrate and nitric acid which
showed the presence of Chlorine, Bromine and Iodine. And the presence of Oxygen was also
identified by adding Ferrox Paper in test tubes containing Toluene, Ethanol and Water and only
Ethanol and Water showed a deep red precipitate indicating the presence of Oxygen. All in all,
this experiment was successful and met the objectives. Each substance was identified and the
experiment with little to no problems. This experiment could have been improved by more careful
reading of the lab manual, using certain lab equipment when it is called for, and multiple trials.
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