5. CoS and NiS dissolve quite slowly in HCl.

A black precipitate at this point, which dissolves only

when HNO3 is added to the mixture, indicates the presence of nickel or cobalt or both.
6. A large excess of Na2O2 is to be avoided. The hydroxides of iron, cobalt, and nickel may be
dispersed to some extent in a strongly basic solution, causing interference with the test for
aluminum and zinc ions. Sufficient Na2O2 should be added to produce a bubbling action for 1min.
7. The Na2O2 is added for the purpose oxidizing the chromite ion to the chromate ion. At the same
time, ferrous and cobaltous hydroxides are oxidized to ferric and cobaltic hydroxides. Manganous
hydroxide is oxidized to hydrated manganese dioxide.

ANALYSIS OF GROUP IIIA CATIONS

Procedure 9. Separation and Identification of Group IIIA Cations. Centrifugate from Procedure 8
contains aluminate, chromate, and zincate ions. Add 10 drops of saturated NH4Ac, then 3F HAc until
acid. Now add 3F ammonia until solution is decidedly ammoniacal. (1) Centrifuge.

Residue may be aluminum
hydroxide. Wash with 10 drops of
water and discard washings. Add 3F
HCl, drop by drop, until residue
dissolves. Add 3 drops of saturated
NH4Ac and 3 drops of aluminon;
then make decidedly ammoniacal
with 3F NH3. Allow mixture to
stand 2 min, then centrifuge.
Separation of a red precipitate
confirms presence of ALUMINUM
ION. (2)
Centrifugate may contain CrO4- and Zn(NH3)4++. (3) Add 1F
Ba(Ac)2 until precipitation is complete. Centrifuge.
Residue may be BaCrO4 and Centrifugate may contain
BaSO4. (4) Add 10 drops of 3F Zn(NH3)4++ ion. Acidify
HCl, and warm 1 min in water solution with 3F HAc, add 5
bath. Centrifuge and discard drops of thioacetamide
white residue. Place 2 drops of solution and place in boiling
centrifugate upon a piece of filter water bath for 5min.
paper. Add 2 drops of H2O2. Formation of a white
Formation of a blue color which precipitate confirms presence
fades rapidly confirms presence of ZINC ION. If precipitate is
of CHROMIUM ION. (5) not white, consult note (6).

NOTES ON THE ANALYSIS OF GROUP IIIA CATIONS

1. The precipitation of aluminum hydroxide is practically complete in the buffered ammonia-

ammonium acetate solution. In this solution, zinc is not precipitated as the hydroxide but is held
in solution as the soluble complex ion, Zn(NH3)4++.
2. “Aluminon” is the coined name for the ammonium salt of aurintricarboxylic acid. The organic
dye forms a red-colored lake with aluminum hydroxide. This test is specific for aluminum under
the conditions described.
3. The solution must be yellow if chromium is present. The color can best be observed by looking
down through the solution contained in a test tube.
4. Any sulfide ions in the solution are converted to sulfate ions by the action of sodium peroxide.
The sulfate ions are precipitated by barium ions as acid-insoluble BaSO4.
5. The addition of hydrogen peroxide to an acid solution of a chromate produces a blue coloration
due to the formation CrO5. This compound is unstable, decomposing rapidly with an evolution of
oxygen, accompanied by a fading of the blue color.