Exercise 13

QUALITATIVE ANALYSIS OF GROUP B CATIONS

(Hydroxides Insoluble in Ammonium Hydroxide)

I. Objectives
1. I must learn to demonstrate the effect of pH on the separation of ions.
2. I must learn to apply the principles pf solubility equilibrium on the separation of Group B
ions from each other.
3. I must learn to apply buffer, complex ion formation and oxidation-reduction principles on
the separation of ions.
II. Modifications in the Procedures:

(!) PRECAUTIONS:
WARNING: THE EXPERIMENT WILL USE 6 M NH3, 6 M NaOH, AND 6 M HCl

WASTE MANAGEMENT: Cr3+ - containing waste ⟶ D405

MNO4- - containing waste ⟶ E501
FeSCN2+ - containing waste ⟶ D499
Bi - containing waste ⟶ D499

III. Results:

Ions present in solution: __________________

__________________
__________________

Sample Reactant/ Net Ionic Equation Observations Conclusions

Action Involved
CA1 - Adding 6 M Bi3+(aq) + NH4OH(aq)
(Cations NH3 dropwise Bi(OH)3(s) + NH4+(aq)
of Groups until neutral Fe3+(aq) + NH4OH(aq)
B-E from - Adding 12 Fe(OH)3(s) + NH4+(aq)
Group A drops of 6 M Mn2+(aq) + NH4OH(aq)
Analysis) NH3 Mn(OH)3(s) + NH4+(aq)
10 drops) - Centrifuge Cr3+(aq) + NH4OH(aq)
and decant Cr(OH)3(s) + NH4+(aq)
supernatant
liquid
PB1a - Adding 10 Mn(OH)2(aq) + H2O2(aq)
{white drops of 6 M MnO2(s) + 2H2O(l)
Bi(OH)3, NaOH and 2
red drops of 3% Cr(OH)2(aq) + OH-(aq) +
brown H2O2 H2O2(aq) CrO42-(aq)
Fe(OH)3, -Stir and allow
pale pink to stand for 2
Mn(OH)2, minutes.
Cr(OH)3} - Centrifuge
 - Decant
supernatant
liquid
PB1a
{Bi(OH)3, -Adding 10
Fe(OH)3, drops of NaOH
Mn(OH)2} and 2 drops of
H2O2
- Stir and allow
stand for 2 min.
-Centrifuge
- Decant
CB1 supernatant
(Groups liquid
C-E)
- Combine the
centrifugates
- Label as CB2

PB2 - Adding 2 mL Bi(OH)3(s) + 3H3O+(aq)

{Bi(OH)3, dH2O, stir and Bi3+(aq) + 6H2O(l)
Fe(OH)3, heating for 10 Fe(OH)3(s) + 3H3O+(aq)
Mn(OH)2} minutes Fe3+(aq) + 6H2O(l)
- Centrifuge MnO2(s) + 4H3O+(aq)
- Decant and Mn4+(aq) + 6H2O(l)
discard
supernatant
liquid
- Washing
- Adding 6
drops of 6 M
HCl
- Stir, heat for
two minutes
- Discard any
precipitate
CB3 4 drops of Mn4+(aq) + 3H2O2(aq)
{Bi3+, CB3 Mn2+(aq) + 2O2(aq) +
Mn4+, - Adding 2 2H3O+(aq)
Fe3+} drops of H2O2 Mn4+(aq) + 4H3O+(aq) + BiO3-
Test - Adding a (aq) Bi3+(aq) + MnO4-(aq)
Solution pinch of solid + 3H2O(l) + 3H2(g)
NaBiO3
- Centrifuge
MnO4- purple
sol’n

2 drops of
CB3
- Adding 3
drops of KSCN
 FeSCN2+
“blood-red
solution”

2 drops of
CB3
- Adding 10
drops of NaOH
- Adding a
pinch of solid
SnCl2
-Centrifuge
Bi black
precipitate

CB2 - Heating in 2CrO42-(aq) + 2H3O+(aq)

{CrO42-} boiling water Cr2O72-(aq) + 3H2O(l)
bath
- Cooling for
two minutes in
a cold-water
bath
- Adding HCl
dropwise until
acidic
- Adding
NaHCO3
dropwise until
neutral
- Discard any
precipitate
CB4 - 2 drops of CB4 Cr2O72-(aq) + H2O2(aq) +
{Cr2O72-} - Adding HCl 2H3O+(aq) + 2Cl-(aq)
dropwise until 2CrO5(aq) + 2Cl-(aq) + H2O(l)
acidic 4CrO5(aq) + 12H3O+(aq)
- Adding 1 drop 4Cr3+(aq) + 18H2O(l)
of H2O2 + 7O2(aq)

CrO5 blue
color that
decomposes
quickly
IV. Answers to Questions
1.) What would happen if you used NH3/H2O2 instead of NaOH/ H2O2 in PB1?

2.) Why can’t the portion of the test solution tested for Mn2+ also be used to test for Bi3+?