SEPARATION AND IDENTIFICATION OF GROUP 3A

CATIONS

Discussion:

All the Group 3A cations form insoluble hydroxides in a basic solution.

The addition of ammonia to this solution raises the pH to about 9 and causes the
ions to precipitate out as hydroxides. The addition of NH4Cl and NH4OH
containing Group 3A cations results in the precipitation of aluminum hydroxide,
chromium hydroxide and ferric hydroxide.

In the scheme of this activity, the cations of Group 3A must be free of

sulfides. Soluble ammonia complexes can be decomposed by addition of acid. In
the presence of a strong base, the addition of an oxidizing agent such as hydrogen
peroxide converts chromium to its soluble trivalent state as well as aluminum.
Ferric ions are not affected by this as it is not amphoteric. This gives way to the
separation of iron, which is an insoluble hydroxide, from the other Group 3A
cations in the mixture.

In the addition of a salt of the weak base NH3 to the mixture of chromium
and aluminum ions, the chromate ion is converted to dichromate ions in slightly
basic solution and re precipitates the hydroxide of aluminum. Dichromates are
generally more soluble than chromates. It is by this principle that chromium ions
can be separated from aluminum ions.
PROCEDURE:

1. Transfer 1 ml of the sample to a test tube. Add 15 drops of 6N NH4Cl. Add

concentrated NH4OH until mixture is alkaline. When the mixture is already
alkaline, add 2 drops of concentrated NH4OH in excess. Add 10 drops 3%
H2O2, and then add 6M NaOH solution dropwise until the precipitate becomes
reddish brown. You may notice the supernatant liquid becoming yellow. Do not
dissolve all the precipitate. Warm the mixture in a water bath for 5 minutes.
Centrifuge the mixture. Label the centrifugate as C1 and the precipitate as P1.

To P1: Confirmation of Fe3+: To C1:

Wash twice with water and discard Add 10 drops of 3N NH4NO3, and
washings. Dissolve the precipitate using verify if precipitation occurs. If no
3N HCl and the add 10 drops of water. precipitation happens, keep adding 3N
Add 3 drops of KCNS. Formation of a NH4NO3, until a notable precipitate is
deep red solution confirms the seen. Proceed to Step 2.
presence of Fe3+.
7. Centrifuge C1. Label the precipitate as P2 and the centrifugate as C2.

To P2: Confirmation of Al3+: To C2: Confirmation of Cr3+:

Dissolve precipitate with 3N HCI while Add 3N HAc until acidic. Add 5 drops
heating in a water bath. Add 10 drops of PbSO4. Formation of a yellow
of NH4Ac and stir while hot. Remove precipitate confirms the presence of Cr.
from water bath and cool. Add 5 drops
aluminum and then add 3N NH4OH.
Allow mixture to stand for 5-10
minutes. Formation of a red precipitate
or "red lake" confirms the presence of
Al3+.