TITLE :

THEORY :

Unlike covalent compounds, which can be identified using physical properties like
boiling point and refractive index, ionic compounds are more appropriately identified with their
chemical properties. In the qualitative analysis procedure, the chemical properties of an
unknown substance are determined by systematically reacting the unknown with a number of
different reagents. By predetermining what the particular reaction will produce if a specific ion
is present, the ions that actually are in the solution can be identified. For example, if a reaction
is known to produce a precipitate if ion A is present and a precipitate is formed when the
reaction is run, then ion A may be present in solution (there may be, and usually are, other
ions that will also precipitate with a particular reagent). If no precipitate is formed when the
reaction is run, then ion A is clearly not present in the unknown solution and a different reaction
will have to be run to determine what ions are present. 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.

Qualitative analysis is a method of Analytical chemistry that deals with the

determination of elemental composition of inorganic salts. It is extremely useful to know how
to detect the presence of specific ions in an aqueous solution. It is mainly concerned with the
detection of ions in an aqueous solution of the salt. The common procedure for testing any
unknown sample is to make its solution and test this solution with various reagents for the ions
present in it. Testing with various reagents gives characteristic reaction of certain ions, which
may be a colour change, a solid formation or any other visible changes. There are separate
procedures for detecting cations and anions, called the Cation Analysis and Anion Analysis.
In this experiment, we will do the cation analysis for metal oxide.

The qualitative analysis of ions in a mixture must follow a scheme that can be
summarized as follows

AIM :

To identify the cation in metal oxide compounds.

PROBLEM STATEMENT :

What is the cation that contained in a metal oxide compound?

MATERIAL :
Sample 1 (S1), Sample 2 (S2), Hydrochloric acid, Nitric acid, Ammonium solution, Sodium
hydroxide, Potassium thiocyanate and distilled water.

APPARATUS :

Beaker, Test tube, test tube rack, Bunsen burner, spatula, tripod stand, wire gauze, glass rod,
filter paper and filter funnel.

PROCEDURES

A. Procedures to Test S1

1. The appearance of the compound is observed.

2. One small spatula of the S1 compound is added into a beaker contained water and
stirred.

3. 30ml of nitric acid solution is heated and excess amount of S1 is added into the
solution to form a salt solution.

4. The concentrated salt solution is filtrated.

5. About 5 ml of salt solution is placed into a test tube and a few drops of NAOH is
added. The solution is stirred. Then, excess of NAOH is added into the solution.

6. After that, about 5 ml of salt solution is placed into a test tube and a few drops of
Ammonium is added. The solution is stirred. Then, excess of Ammonium is added
into the solution.

7. All of the observations are recorded.

B. Procedures to Test S2

1. The appearance of the compound is observed.

2. One small spatula of the S2 compound is added into a beaker contained water and
stirred.

3. 30ml of hydrochloric acid solution is heated and excess amount of S2 is added into
the solution to form a salt solution.

4. The concentrated salt solution is filtrated.

5. About 5 ml of salt solution is placed into a test tube and a few drops of NAOH is
added. The solution is stirred.
 6. After that, about 5 ml of salt solution is placed into a test tube and a few drops of
Ammonium is added. The solution is stirred.

7. After that, about 5 ml of salt solution is placed into a test tube and a few drops of
Potassium thiocyanate is added. The solution is stirred.

8. All of the observation are recorded.

OBSERVATION AND ANALYSIS :

A. Observation and Analysis for S1

Observation Analysis

The S1 compound is a black powder The compound maybe Copper(II)

oxide, CuO , Iron(II) oxide, FeO or
Manganese(IV) oxide, MnO2

Insoluble in water Group 1 metals are absent in S1

compound.

Soluble in HNO3 and form a blue Copper (II) ion are present.
solution.

Blue precipitates formed when NaOH is Copper (II) ion are present.
added.

Dark blue solution is formed when

excess of NaOH is added.

Blue precipitates formed when NH4 is Copper (II) ion are present.
added.

Dark blue solution is formed when

excess of NH4 is added.
 B. Observation and Analysis for S2

Observation Analysis

The S2 compound is a reddish brown The S2 compound maybe Ferum(III)

powder. Oxide

Insoluble in water. Group 1 metals are absent

Soluble in HNO3 and form a light red The presence of ferum(III) ion.
solution.

Remain unchanged when NaOH is There is no reaction happen.

added

Remain unchanged when NH4 is added There is no reaction happen.

The solution turned to dark red when Ferum (III) Ions are present.
KSCn is added.

RESULT :

1. S1 compound is Copper (II) Oxides. The cation is Copper (II).

2. S2 compound is Ferum (III) Oxides. The cation is Ferum (III).

DISCUSSION :

For this experiment, we are given two unknown compound, S1 and S2. S1 and S2 are
metal oxide, so we need to do a qualitative test to identify the cation contained in S1 and S2.
Firstly, for S1, I observed the appearance of the compound. The compound is in a powder
form which is black in colour. So, based on its appearance, the compound maybe The
compound maybe Copper(II) oxide, CuO , Iron(II) oxide, FeO or Manganese(IV) oxide, MnO2.
Then, I add the compound into the water and stir it to test the solubility of the compound. S1
is insoluble in water, so the metal cation in S1 is not a group 1 metals because all of metal
oxide are insoluble in water except group 1 metal oxide. To test the presence of cations, they
must be in liquid or aqueous form. So, I add S1 excessively into heated nitric acid. The reaction
will produce a nitrate salt and water. S1 is added excessively into the acid to make sure that
all of the acids are completely react with S1. Then, the salts solution that produced will be
filtrated. After that, a few drops of NaOH are added into the nitrate solution and blue precipitate
form. Based on this observation, hypothesis that can be made is Copper (II) ion, Cu2+ is
present. To prove the hypothesis, excess of NaOH is added and a dark blue solution formed.
So, it shows that Copper (II) ion is present. Then, I try to test again the solution by adding
ammonium solution and blue precipitate was formed. Next, I add excess of ammonium
solution and it formed a dark blue solution. From all the test that I have done, It is proven that
the cation in S1 is Copper (II). So, S1 is Copper (II) Oxide.

To test the cation in S2, first of all, I observed the appearance of S2. S2 is a reddish
brown powder. Based on this observation, hypothesis that can be make is that, S2 is Ferum
(III) oxide because it is the only metal oxide that have his colour. So, to confirm whether the
hypothesis is acceptable or not, I need to do the qualitative test. Firstly, I add the compound
into the water and stir it to test the solubility of the compound. S2 is insoluble in water, so the
metal cation in S2 is not a group 1 metals because all of metal oxide are insoluble in water
except group 1 metal oxide. To test the presence of cations, they must be in liquid or aqueous
form. So, I add S2 excessively into heated nitric acid. The reaction will produce a nitrate salt
and water. S2 is added excessively into the acid to make sure that all of the acids are
completely react with S2. Then, the salts solution that produced will be filtrated. Next, a few
drops of NaOH are added into the solution. However, there was no precipitate formed and
remain unchanged. Then, when a few drops of ammonium solution is added into the solution,
there was also no precipitate formed and remain unchanged. From these observation where
the solution remain unchanged, the cations that present maybe the ions from group 1 metals.
But, we know that S2 is not a group 1 metal compound because it is insoluble in water.
Besides, the group 1 metal oxides is normally a white colour powder. So, to test the compound,
I added Potassium Thiocyanate into the solution and it formed a dark red solution. Formation
of dark red solution proved that, Ferum (III) ion is present in the solution. So, S2 is Ferum (III)
Oxide. Back to the observation when we add the NaOH and ammonium solution, the solution
is remain unchanged when actually if Ferum(III) ion is present, browm precipitate will formed.
So, I assume that the concentration of Ferum(III) ion in the nitrate solution is too low so that,
the changed that happen to the solution is not clearly seen.

During this experiment, a few of precaution steps have been take such as I used
spatula to add the compound into the water or acid to avoid a direct contact. Besides, I add
excess of S1 and S2 into the acid to make sure that all of the acids are completely react. There
is a weakness when I carry out this experiment. For S2, when I add excess of S2 into the
heated nitric acid, there were precipitate formed. So, I thought that it was already saturated
when actually, S2 is not completely react with the acid yet. As a result, solution that has been
filtrated contain low concentration of ferum(iii) ion and the solution is slightly acidic because
HNO3 is not completely react with S2.

CONCLUSION :

As the conclusion, S1 compound is Copper(ii) Oxide where the cation is Copper(II), Cu2+
while S1 compound is Ferum(III) oxides where the cation is Ferum(III), Fe3+.