The Detection of ”Chloride“

Radical in Inorganic Salts

Description:
The chloride radical is among the second group of the acidic radical in
which concentrated sulphuric acid is used as group reagent.
In this experiment, the salt is dissolved in water to test its solubility in water
then it will be tested with concentrated sulphuric acid then we will do
confirmatory tests with silver nitrate and lead acetate then chromyl chloride
test will be carried out to confirm the presence of chloride radical in the salt.

Learning objective:
- To test for the chloride radical in inorganic salts.
- Students understand various tests to identify the anion present in a given
salt.
- Students understand the chemical reactions and their balanced equations
that takes place during each test.
- Students acquire the skill to perform the experiment in the real lab once
they understand different steps in the procedure.

Tools & materials:

- Sodium chloride salt.
- Test tubes.
- U shaped tube.
- Spatula.
- Distilled water.
- Concentrated sulphuric acid.
- Ammonium hydroxide solution.
- Glass rod.
- Silver nitrate solution.
- Lead acetate solution.
- Potassium dichromate powder.
- Sodium hydroxide solution.
- Dilute acetic acid.
- Bunsen flame.
Procedure:
Step 1: Select “NaCl” salt from the salt tab
Observation: The salt is in shape of colorless crystals.

Step 2: Solubility test:

Place a small amount of the salt in a test tube by the spatula then add (1-2)
mL of water then shake the test tube well.

Observation: soluble in water

Step 3: (Concentrated sulphuric acid test)

Put a small amount of the salt in a test tube by the spatula then add drops
of concentrated sulphuric acid then moisten a glass rod with ammonium
hydroxide then hold it at the tube’s nozzle.

Observation: dense white fumes evolve.

Result: Colorless Hydrogen chloride gas evolves which reacts with the
ammonium hydroxide at the tube’s nozzle resulting in the evolution of
dense white fumes of ammonium chloride.
↓
NaCl + H2SO4 → NaHSO4 + HCl
Sodium bisulphate

NH4OH + HCl → NH4Cl + H2O

Step 4: (Confirmatory test 1)

Dissolve a small amount of the salt in (1-2) mL of water in a test tube then
add drops of the confirmatory test reagent Silver nitrate

Observation: White precipitate is formed.

Result: The formation of white precipitate of silver chloride which is soluble

in ammonium hydroxide.

NaCl + AgNO3 → AgCl ↓ + NaNO3

White precipitate
Step 5: (Confirmatory test 2)
Dissolve a small amount of the salt in (1-2) mL of water in a test tube then
add drops of confirmatory test reagent Lead acetate.

Observation: White precipitate is formed.

Result: The formation of white precipitate of lead chloride.

2 NaCl + Pb(CH3COO)2 → PbCl2 + 2 CH3COONa

Step 6:( Chromyl chloride test )

Prepare a small amount of sodium hydroxide in a test tube.
In another test tube place a small amount of the salt then add small amount
of potassium dichromate powder to the salt using a spatula then mix the
content of the test tube using glass rod then add drops of concentrated
sulphuric acid to the mixture using dropper then heat the mixture on the
Bunsen flame.

Observation: Red vapor evolves.

Then pass the red vapor to the tube containing sodium hydroxide.

Observation: yellow solution is formed.

Then add a small amount of acetic acid to the yellow solution then add few
drops of lead acetate using dropper.

Observation: yellow precipitate is formed.

Result: Sodium chloride salt reacts with potassium dichromate and conc.
sulphuric acid forming red fumes of chromyl chloride which reacts with
sodium hydroxide to form yellow solution of sodium chromate. Sodium
chromate reacts with lead acetate in presence of dil. acetic acid to form
yellow precipitate of lead chromate.

4NaCl + K2Cr2O7+ 3H2SO4 → 2Na2SO4 + K2SO4 + 2CrO2Cl2 + 3H2O

chromyl chloride
(Red fumes)

CrO2Cl2 + 4 NaOH → Na2CrO4 + 2H2O + 2NaCl

Sodium chromate

Na2CrO4 + (CH3COO)2Pb → PbCrO4 + 2CH3COONa

lead chromate
(yellow precipitate)
Conclusion:
The presence of chloride ion is confirmed.