ORDINARIA, SHERWIN D.

ANALYTICAL CHEMISTRY -
LAB
BSMLS 1G

FLOWCHART
GROUP III ANIONS
LAB ACTIVITY NO. 6
 UNKNOWN SAMPLE
+ 15 drops of Cd(Ac)2
centrifuge

Wash twice with hot water

Discard washings

FIRST PORTION SECOND PORTION THIRD PORTION

PRECIPITATE CENTRIFUGATE
(Sulfide ions, Ferrocyanide
Place in depression of a
+ 3 drops of 3M HCl ions, Ferricyanide ions)
spot plate
Moisten strip of filter paper with 0.5 M Pb(Ac)2 + 1 drop of 3M HCl
Cover the mouth of test tube using the strip DISCARD
+ 1 drop of 1M FeCl2

BROWN /BLACK
DARK BLUE
COLOR OF THE FILTER
PRECIPITATE
PAPER
(PRUSSIAN BLUE)

NO NO
- Ferricyanide
END -Fe(CN) 6
4-
ions ions
END END

Place in a depression of a spot

plate
Dissolve with 1 drop of 3M HCl
+ 3 drops of H2O
+ 1 small crystal of FeSO4

(TURNBULL BLUE)

YES NO YES + NO YES

+ Sulfide - Sulfide ion +Ferrocyanide
+ Ferricyanide
ions ions Ferrocya ions
nide ion

ORDINARIA, SHERWIN D. ANALYTICAL CHEMISTRY -LAB

BSMLS – 1G

ANALYSIS OF GROUP III ANIONS

Lab Activity No. 6

 Group III anions are those ions whose calcium and barium salts are soluble but whose cadmium salts are
insoluble in neutral or basic solutions. The test for the three anions are made in three portions with precipitation
be cadmium ions that is fairly complete.

 Precipitate

The precipitate for this activity is washed thoroughly with hot water to remove any contamination of
thiocyanate ion because this ion will interfere with the test for ferrocyanide since both ions react with ferric
(identification reagent).

 Precipitation of Group III Anions

The three anions in this are precipitated by a reagent called Cadmium Acetate. The different color of the
precipitate is an indication of its composition.

Sulfide:(yellow)

Ferrocyanide: pale yellow (almost white).

Ferricyanide: (orange)

 1st portion ( Detection of Sulfide Ion )

The reagent used to confirm the sulfide ion is the hydrochloric acid. The cadmium sulfide is dissolved because of
its solubility to 3M HCl.

S2- + Cd2 Cd 3-+ H2S + 2 H2O

The sulfide together with the strip of moisten filter paper with 0.5 Pb(Ac use)2 causes the change in color to
black/brown – positive indicator. Due to formation of Pbs.

Pb(Ac)2 + H2S PbS + 2 HAc

 2nd portion ( Detection of Ferrocyanide Ion)

 The reagent used to confirm the ferrocyanide ion is the hydrochloric acid. The cadmium ferrocyanide is dissolved
in 3M HCl.

Cd 2Fe(CN) + 2 H2O H 2Fe(CN) + 2Cd3+ + 2 H2O

The ferrocyanide ion reacts with ferric ion to produce the dark blue precipitate called Prussian blue.

3 H 2Fe(CN)6 + 4 Fe2+ + 6 H2O Fe [Fe(CN) 6]3+ 6 H2O

 3rd portion ( Detection of Ferricyanide Ion )

The reagent used to confirm the presence of ferricyanide ion is the hydrochloric acid. The cadmium ferricyanide
ion is dissolved in 3M HCl.

Cd 3[Fe(CN)6]2+ 2 H2O 2 HFe(CN) + 3 Cd 3+ + 2 H2O

The ferricyanide ion reacts with ferrous ions to produce dark blue precipitate called Turnbull's blue.

HFe(CN) 6 + 4 Fe2++ 6 H2O H 2Fe(CN)6 + Fe2++ H2O

FLOW CHART : GROUP III ANIONS
ORDINARIA, SHERWIN D. ANALYTICAL CHEMISTRY -LAB

BSMLS – 1G

ANALYSIS OF GROUP III ANIONS

Lab Activity No. 6

Group III anions are those ions whose calcium and barium salts are soluble but whose cadmium salts are
insoluble in neutral or basic solutions. The test for the three anions are made in three portions with precipitation
be cadmium ions that is fairly complete.

 Precipitate

The precipitate for this activity is washed thoroughly with hot water to remove any contamination of
thiocyanate ion because this ion will interfere with the test for ferrocyanide since both ions react with ferric
(identification reagent).

 Precipitation of Group III Anions

The three anions in this are precipitated by a reagent called Cadmium Acetate. The different color of the
precipitate is an indication of its composition.

Sulfide:(yellow)

Ferrocyanide: pale yellow (almost white)

Ferricyanide: (orange)
 1st portion ( Detection of Sulfide Ion )

The reagent used to confirm the sulfide ion is the hydrochloric acid. The cadmium sulfide is dissolved because of
its solubility to 3M HCl.

S2- + Cd2+ Cd3- + H2S + 2H2O

The sulfide together with the strip of moisten filter paper with 0.5 Pb(Ac use)2 causes the change in color to
black/brown – positive indicator. Due to formation of Pbs.

Pb(Ac)2 + H2S. Pbs + 2 HAc

 2nd portion ( Detection of Ferrocyanide Ion)

The reagent used to confirm the ferrocyanide ion is the hydrochloric acid. The cadmium ferrocyanide is dissolved
in 3M HCl.

Cd2Fe(CN) + 2 H2O H2Fe(CN) + 2Cd3+ + 2 H2O

The ferrocyanide ion reacts with ferric ion to produce the dark blue precipitate called Prussian blue.

3 H2Fe(CN)6 + 4 Fe2+ + 6 H2O Fe [Fe(CN)6]3 + 6 H2O

 3rd portion ( Detection of Ferricyanide Ion )

The reagent used to confirm the presence of ferricyanide ion is the hydrochloric acid. The cadmium ferricyanide
ion is dissolved in 3M HCl.

Cd3[Fe(CN)6]2 + 2 H2O 2 HFe(CN) + 3 Cd 3+ + 2 H2O

The ferricyanide ion reacts with ferrous ions to produce dark blue precipitate called Turnbull's blue.

HFe(CN)6 + 4 Fe2+ + 6 H2O H2Fe(CN)6 + Fe2+ + H2O

FLOW CHART : GROUP III ANIONS