Experiment 8: Identification of metal ions and inorganic compounds in

aqueous solution

Objective:
To identify the inorganic compounds by their chemical reactions.

Introduction:
Inorganic qualitative analysis is the unambiguous identification of cations (and/or
anions) present in solution. Unique tests for all ions in the possible presence of
all others are virtually impossible to devise. Many tests give similar results with
different cations. However, if a solution is treated to separate ions into smaller
groups, identification is simplified. The most common way to subdivide cations
into smaller groups is by selective precipitation, in which a small group of cations
is precipitated chemically. The precipitate can then be physically separated from
the remaining cations in solution by centrifuging. The precipitate (insoluble solid)
settles out and the solution (supernatant liquid) is decanted into another
container. In this way the initial large group can be separated into smaller groups
until a definitive test can be performed to verify the presence or absence of each
specific cation. It is important to realize that many chemical reactions do not go to
completion. The extent to which a reaction occurs depends on the magnitude of
the equilibrium constant, Ksp for the reaction and the concentrations of reagents
present. Equilibria can be shifted by adding or removing reagents and by altering
the physical conditions in accordance with Le Châtelier's principle. In this
analysis scheme, you will use various reagents to force precipitation to occur,
dissolve sparingly soluble compounds or complex particular ions so they will not
interfere with tests for other ions.

Apparatus Needed:
Test tubes, droppers
Chemicals Needed:
0.1 M Ba (NO3)2 solution, 0.1 M Mg(NO3)2 solution, 0.1 M Pb(NO3)2 solution,
0.1 M Co(NO3)2 solution, 0.1M Fe(NO3)3 solution, 0.5M (NH4)2SO4, 0.5M
NH4SCN, 0.5M NaOH solution, 4M NaOH solution, 0.5M NH3(aq) solution, 4M
NH3(aq) solution, 0.5 M CuSO4 solution, 0.5 M Pb(NO3)2 solution, 0.5 M
Zn(NO3)2 solution, 0.5 M BaCl2

Procedures:

A. Identification of metal ions in aqueous solution

1. Obtain five dry test tubes. Label the test tubes 1, 2, 3, 4 and 5.
2. Add four drops of 0.1 M Ba (NO3)2 solution to test tube 1, four drops of 0.1
M Mg(NO3)2 solution to test tube 2, four drops of 0.1 M Pb(NO 3)2
solution to test tube 3, four drops of 0.1 M Co(NO3)2 solution to test
tube 4, and four drops of 0.1M Fe(NO3)3 solution to test tube 5.
3. Record the color of the metal ion solution in each test tube in the results
section.
4. Add four drops of 0.5M (NH4)2SO4 to each of the five test tube in step 2.
Carefully observe the test tube for any evidence of reaction. Record your
observations in the table on the results section. Write the formulas of the
substances formed in this reaction in the results section. If no reaction
occurs, write ‘no change, NC’.
5. Empty the contents of the five test tubes into the waste container.
6. Repeat steps 1 and 2 above, adding four drops of each metal nitrate
solution to separate clean, dry test tubes.
7. Add four drops of 0.5M NH4SCN to each of the five test tubes from steps 6.
Carefully observe the test tubes for any evidence of reaction. Record your
observations in the table on the data sheet. Empty the contents of the five
test tubes into the waste container.
8. Repeat steps 1 and 2, adding four drops of each metal nitrate solution to
separate clean, dry test tubes.

9. Add four drops of the freshly prepared 0.5M NaOH solution (limited OH-
 ions) to each of the five test tubes in step 8. Carefully observe the test
tubes for any reaction. Record your observations in the results section.
Empty the contents of the five test tubes into the waste container.
10. Repeat steps 1 and 2, adding four drops of each metal nitrate solution to
separate clean, dry tubes.

11. Add four drops of 4M NaOH solution (excess OH- ions) to each of the five
test tubes in step 10. Carefully observe the test tubes for any evidence of
reaction. Record your observations in the results section. Empty the
contents of the five test tubes into the waste container.
12. Repeat steps 1 and 2, adding four drops of each metal nitrate solution to
separate clean, dry test tubes.
13. Add four drops of the freshly prepared 0.5M NH3(aq) solution to each of
the five test tubes in step 12. Carefully observe the test tubes for any
evidence of reaction. Record your observation on the data sheet. Empty
the contents of the five test tubes into the waste container.
14. Repeat steps 1 and 2, adding four drops of each metal nitrate solution to
separate clean, dry test tubes.

15. Add four drops of 4M of NH3(aq) solution to each of the five test tubes in
step 14. Carefully observe the test tubes for any evidence of reaction.
Record your observations in the table in the results section. Empty the
contents of the five test tubes into the waste container..
16. Write the balanced net ionic equations for all reactions that occurred in
steps 4-15.
17. Obtain 2 mL of an unknown metal ion solution from your laboratory
instructor. Record the color of the unknown metal ion solution on the data
sheet.
18. Label six clean, dry test tubes as 1, 2, 3, 4, 5 and 6. Add four drops of the
unknown metal solutions to each of the test tubes.
19. Add four drops of 0.5 M (NH4)2SO4 solution to test tube 1. Add four drops
of 0.5M NH4SCN solution to test tube 2. Add four drops of 0.5M NaOH
solution to test tube 3. Add 4 drops of 4M NaOH solution to test tube 4.
Add four drops of 0.5M NH3 solution to test tube 5. Add four drops of 4M
 NH3 solution to test tube 6. Carefully observe the test tubes for any
evidence of reaction. Record your observations in the table on the data
sheet.
20. From your observations of the reactions of the known and unknown metal
ions, identify the unknown metal ion.

B. Identification of inorganic compounds in aqueous solution

1. Develop and carry out a procedure to determine whether double

displacement reactions occur when solutions of the following five
compounds are mixed. Use only four drops of each solution for each
reaction. Record the colours of the solutions listed below.
2. Carefully observe the mixtures in each test tube for any evidence of
reaction. Record your observations in the results section.
3. Obtain an unknown inorganic compound solution and record the color of
the unknown solution.
4. In five separate test tubes, mix four drops of the unknown compound with
each of the test from step 1.
5. Carefully observe the mixtures in each test tube and record the
observations
6. From your observations of the reactions of the known and unknown
inorganic compounds, identify the unknown inorganic compound.

Results:

A. Identification of metal ions in aqueous solution

1. Color of the metal ion solutions

Inorganic compounds Observation(s)

Ba(NO3)2 Colourless
Mg(NO3)2 Colourless
Pb(NO3)2 Colourless
Co(NO3)2 Pale Pink
Fe(NO3)2 Yellow
2. At the top (white space) of each box in the table below, record
your observations (e.g., white precipitate, solutions turns green, etc.).
At the bottom (gray space) of each box, write the formula for the
substances (e.g., precipitates or complex ions) formed when the ions are
mixed. If no reaction occurs, write NC (no changes) in the boxes.

Metal ions
Test Ba2+ Mg2+ Pb2+ Co2+ Fe3+
reagent
(NH4)2SO4 White No change White No change No change
precipitate precipitate
BaSO4 No change PbSO4 No change No change
NH4SCN No change No change No change No change Solution
turns
blood red
No change No change No change No change Fe(SCN)3
0.5M No change White White Blue Brick red
NaOH precipitate precipitate precipitate precipitate
(limited) Ba(OH)2 Mg(OH)2 Pb(OH)2 Co(OH)2 Fe(OH)3
4M NaOH No change White No change Blue Brick red
(excess) precipitate precipitate precipitate
Ba(OH)2 Mg(OH)2 No change Co(OH)2 Fe(OH)3
0.5M NH3 No change No change White Blue Brick red
(aq) precipitate precipitate precipitate
(limited) Ba(OH)2 No change Pb(OH)2 [Co(NH3)6]2+ Fe(OH)3
4M NH3 No change White White Green Brick red
(aq) precipitate precipitate precipitate precipitate
(excess) Ba(OH)2 Mg(OH)2 Pb(OH)2 [Co(NH3)6]2+ Fe(OH)3
 3. Write the balanced net ionic chemical equations for all reactions that occurred.

Metal ions
Test Ba2+ Mg2+ Pb2+ Co2+ Fe3+
reagent
(NH4)2SO4 Ba2++ SO42- No reaction Pb2+ + SO42- → No reaction No reaction
→ BaSO4 PbSO4

NH4SCN No reaction No reaction No reaction No reaction Fe3+ +

SCN- →
Fe(SCN)3
0.5M Ba2+ + 2OH- Mg2+ + 2OH- Pb2+ + 2OH- → Co2+ + 2OH- Fe3+ +
NaOH →Ba(OH)2 → Mg(OH)2 Pb(OH)2 →Co(OH)2 3OH-
→Fe(OH)3
4M NaOH Ba2+ + 2OH- Mg2+ + 2OH- No reaction Co2+ + 2OH- Fe3+ +
→Ba(OH)2 → Mg(OH)2 →Co(OH)2 3OH-
→Fe(OH)3
0.5 M NH3 Ba2+ + 2OH- No reaction Pb2+ + 2NH3 + [Co(H2O)4]2+ Fe3+ +
→Ba(OH)2 3H2O + 2NO3- + NH3 → 3OH-
→Pb2O(NO3)2 + [Co(NH3)6]2+ →Fe(OH)3
H2O + 2NH4+

4 M NH3 Ba2+ + 2OH- Mg2+ + 2OH- Pb2+ + 2NH3 + [Co(H2O)4]2+ Fe3+ +

→Ba(OH)2 →Mg(OH)2 3H2O + 2NO3- + NH3 → 3OH-
→Pb2O(NO3)2 + [Co(NH3)6]2+ →Fe(OH)3
H2O + 2NH4+

4. Color of unknown metal ion solution is Colorless

5. Observation for the unknown metal ion.

SO42- SCN- 0.5M 4M 0.5M 4M

NaOH NaOH NH3 NH3
Unknown No change No change White White No change White
metal ion precipitate precipitate precipitate

No change No change Mg(OH)2 Mg(OH)2 No change Mg(OH)2

6. Identity of the unknown metal ion is Mg2+.

B. Identification of inorganic compounds in aqueous solution

1. Record the colors of the known inorganic compound solutions.

0.5 M NaOH Clear solution

0.5 M CuSO4 Blue solution
0.5 M Pb(NO3)2 Clear solution
0.5 M Zn(NO3)2 Clear solution
0.5 M BaCl2 Clear solution

2. At the top (white space) of each box in the table below, record
your observations (e.g., white precipitate, solutions turns green, etc.).
At the bottom (gray space) of each box, write the formula for the
substances (e.g., precipitates or complex ions) formed when the ions are
mixed. If no reaction occurs,write NC in the boxes.
 BaCl2 Zn(NO3)2 Pb(NO3)2 CuSO4
NaOH Colourless White White precipitate Blue precipitate
Ba(OH)2 precipitate
Zn(OH)2 Pb(OH)2 Cu(OH)2
CuSO4 White precipitate Blue solution White precipitate
BaSO4 No change PbSO4
Pb(NO3)2 White precipitate Colourless
PbCl2 No change
Zn(NO3)2 Colourless
No change

3. Write the balanced net ionic equations for all reactions that occurred.

BaCl2 Zn(NO3)2 Pb(NO3)2 CuSO4

NaOH Ba2+ + 2OH- Zn2+ + 2OH- Pb2+ + 2OH- Cu2+ + 2OH-
→Ba(OH)2 →Zn(OH)2 →Pb(OH)2 →Cu(OH)2
CuSO4 Ba2++ SO42- No change Pb2+ + SO42-
→ BaSO4 → PbSO4
Pb(NO3)2 Pb2+ + 2Cl- No change
→ PbCl2
Zn(NO3)2 No change

NaOH CuSO4 Pb(NO3)2 Zn(NO3)2 BaCl2

Unknown White White Colourless Colourless White
Inorganic precipitate precipitate solution solution precipitate
Compound Pb(OH)2 PbSO4 No change No change PbCl2

Identity of the unknown compound is Pb(NO3)2.

Discussion:

Two experiments are carried out in order to determine the identification of

metal ions and inorganic compounds in aqueous solution. Two unknowns are used
in this experiment and the identification of these unknowns is determined by their
chemical reaction. In these two experiments, for experiment Part A is the
identification of metal ions in aqueous solutions while experiment B is the
identification of inorganic compound in aqueous solution.

There are two reactions involved in these experiments which are precipitation
and double displacement reactions. Most precipitation reactions that occur are single
replacement reactions or double displacement reactions. A double displacement
reaction occurs when two ionic reactants dissociate and bond with the respective
anion or cation from the other reactant. The ions replace each other based on their
charges as either a cation or an anion. If an ion is soluble, then it will remain in its
aqueous ion form. If an ion is insoluble based on the solubility rules, then it will form
a solid with an ion from the other reactant in an equation. If all the ions in a reaction
are shown to be soluble, then no precipitation reaction occurs (2).

A. Identification of metal ions in aqueous solution.

In experiment A, the metal ions such as Ba2+, Mg2+, Pb2+, Co2+ and Fe3+ are
tested. The solutions used are Ba(NO3)2, Mg(NO3)2, Pb(NO3)2, Co(NO3)2 and
Fe(NO3)3 which are tested in their aqueous state. All of these metal ions are in
nitrate solution since all nitrate salt is soluble in water which enables their metal ions
easier to separate and to be collected. The test reagent that is used in this
experiment includes 0.5M (NH4)2SO4, 0.5M NH4SCN, 0.5M NaOH (limited), 4M
NaOH (excess), 0.5M NH3(aq) (limited) and 4M NH3(aq) (excess).

Based on the result, during the test of the metal ion with 0.5M (NH 4)2SO4,
Ba2+, Mg2+ and Pb2+ produced white precipitate and Fe3+ with brown precipitate
whereas Co2+ shows no reaction. These indicates that, when Ba2+, Mg2+, Pb2+ and
Fe3+ reacts with aqueous ammonium solutions it will react with ions from the
reactants such as BaSO4, MgSO4, PbSO4 and Fe(SO4)3 to produce precipitate and
form a solid.
 As for the test of the metal ion with 0.5M NH4SCN, only Fe3+ shows reaction
by forming blood red solution. This shows Fe3+ reacts with ammonium thiocynate, it
will produce Fe(SCN)3.

During the test of the metal ion with 0.5M NaOH aqueous, white precipitate is
formed for Mg2+ and Pb2+, while Co2+ with blue precipitate and Fe3+ with brick red
precipitate. However, the precipitate are insoluble when Mg2+, Co2+ and Fe3+ reacts
with excess NaOH (4M) except for Pb2+. As for Pb2+, the white precipitate is soluble
in excess NaOH.

For the test of the metal ion with 0.5M NH3 aqueous, Pb2+ formed white
precipitate, Co2+ with blue precipitate and Fe3+ with brown precipitate. However,
when Mg2 reacts with excess NH3 (4M), white precipitate is formed and it is insoluble
As for Co2+, it forms blue precipitate which turns into brown solution overtime..

This experiment is also conducted with unknown metal ion A. The result
show that this unknown formed white precipitate 0.5M NaOH, 4M NaOH and 4M
NH3(aq). Thus, the unknown metal ion A is expected to be Mg2+.

B. Identification of inorganic compounds in aqueous solution

There are two general situations in which qualitative analysis is used - in the
identification of a simple salt, or the identification of multiple cations in a solution. For
experiment B, the identification of inorganic compound in aqueous solution is an
example of qualitative analysis through the identification of a simple salt. Some salts
are soluble in water and some are not. Insoluble salts tend to form a precipitate and
this can be obtained by reacting two soluble salts through the process of double
displacement reaction. A double displacement reaction occurs when two ionic
reactants dissociate and bond with the respective anion or cation from the other
reactant. The ions replace each other based on their charges as either a cation or an
anion. This can be thought of as "switching partners," that is, the two reactants "lose"
their partner and form a bond with a different partner.
 There are the general solubility rules for inorganic compounds, primarily
inorganic salts. In this experiment, we use the solubility rules to determine whether a
compound will dissolve or precipitate. General solubility rules:
o All nitrates are soluble.
o Practically all sodium, potassium, and ammonium salts are soluble.
o All chlorides, bromides, and iodides are soluble except those of silver,
mercury(I), and lead(II).
o All sulfates are soluble except those of strontium, barium, and lead(II), which
are insoluble, and those of calcium and silver which are moderately soluble.
o All carbonates, sulfites, and phosphates are insoluble except those of sodium,
potassium, and ammonium.
o All sulfides are insoluble except those of the alkali metals, the alkaline earth
metals, and ammonium.
o All hydroxides are insoluble except those of the alkali metals. The hydroxides
of calcium, strontium, and barium are moderately soluble. Ammonium
hydroxide does not exist; ammonium hydroxide is a misnomer for aqueous
ammonia, NH3(aq).

In experiment B, the inorganic compound used includes NaOH, BaCl 2,

Zn(NO3)2, Pb(NO3)2 and CuSO4. Based on the result, NaOH reacted with BaCl2 and
produces a colourless solution, CuSO4 reacted with BaCl2 and produces white
precipitate, Pb(NO3)2 reacted with BaCl2 and produces white precipitate and
Zn(NO3)2 reacted with BaCl2 and produces a colourless solution. NaOH reacted with
Zn(NO3)2 produces white precipitate, CuSO4 reacted with Zn(NO3)2 produces a blue
solution and Pb(NO3)2 reacted with Zn(NO3)2 produces a colourless solution. NaOH
reacted with Pb(NO3)2 produces white precipitate and CuSO4 reacted with Pb(NO3)2
produces white precipitate and blue solution. Lastly, NaOH reacted with CuSO4
produces blue precipitate. This experiment is continued with unknown compound B,
this unknown gives out white precipitate when reacting with NaOH and BaCl2, blue
solution when reacting with CuSO4 and colourless solution when reacting with
Zn(NO3)2 and Pb(NO3)2. The unknown compound B is expected to be Pb(NO3)2.

Conclusion:

In conclusion, the unknown metal ion A is Mg2+ and the unknown compound B is
Pb(NO3)2.

Questions:

1. In part A of this experiment, all of the test metal and unknown metl
ion solutions were prepared from metal nitrate slats. Why were metal
nitrate salts used to prepare these solutions?

Metal nitrate salts used to prepare these solutions because all nitrate salt is
soluble in water which enables their metal ions easier to separate and to be
collected.

2. Write balanced formula unit and net ionic equations for each of the
following chemical reactions in aqueous solution. If no reaction occurs,
write NC.
a. copper (II) sulfate + lead (II) nitrate copper nitrate (II) + lead (II) sulfate
 CuSO4 (aq) + Pb(NO3)2 (aq)  Cu(NO3)2 (aq) + PbSO4 (s)
 Pb2+ + SO42- → PbSO4

b. zinc nitrate + ammonium thiocynate  NC

c. iron (III) nitrate + ammonium thiocynate  iron(III) thiocynate + ammonium

nitrate

 Fe(NO3)3 (aq) + NH3SCN (aq)  Fe(SCN)3 (aq) + NH3NO3 (aq)

 Fe3+ + SCN-  Fe(SCN)3
d. barium chloride + potassium sulfate  potassium chloride + barium sulfate
 BaCl2 (aq) + K2SO4 (aq)  2KCl (aq) + BaSO4 (s)
 Ba2+ + SO42-  BaSO4

e. magnesium nitrate + excess aqueous ammonia  Magnesium hydroxide +

ammonium nitrate
 Mg(NO3)2(aq) + 2NH4OH(aq)  Mg(OH)2 (s) + 2NH4NO3 (aq)
 Mg2+ + 2OH- → Mg(OH)2

f. barium nitrate + limited sodium hydroxide barium hydroxide + sodium nitrate

 Ba(NO3)2 (aq) + 2NaOH (aq) → Ba(OH)2(aq) + 2Na(NO3) (aq)
 Ba2+ + 2OH- → Ba(OH)2

g. potassium hydroxide + cobalt (II) nitrate  potassium nitrate + cobalt hydroxide

 KOH (aq) + Co(NO3)2 (aq) → 2KNO3 (aq) + Co(OH)2 (s)
 Co2+ (aq) + 2OH- (aq) → Co(OH)2 (s)

References:

1) http://www.docbrown.info/page13/ChemicalTests/ChemicalTestsc.htm
2) http://www.gcsescience.com/f18.htm
3) http://www.gcsescience.com/f17.htm
4) http://chemlab.truman.edu/CHEM131Labs/QualAnalysis.asp
5) http://chemwiki.ucdavis.edu/Inorganic_Chemistry/Reactions_in_Aqueous_Sol
utions/Precipitation_Reactions