EXPERIMENT 1

TITLE: Qualitative Analysis Of Cations: Ca2+, Ba2+, Mg2+, Zn2+ and Al3+

OBJECTIVE:

To identify the cations in known and unknown samples.

To construct a logical flow chart for identifying the components of a mixture of

unknown cations.

INTRODUCTION:

In this experiment we will study about qualitative analysis of cations: Ca2+, Ba2+,
Mg2+, Zn2+ and Al3+. Qualitative analysis is an analytical procedure in which the question
what is present? is answered. In a systematic qualitative analysis scheme, each substance
present is separated from the other substances. Then a confirmatory test is used to prove
that the isolated substance is expected one. As the name indicates, qualitative analysis is
not concerned with the quantity of substance present, but rather is simply used to confirm
its existence. It is mainly focused on detecting ions in an aqueous solution. The solution is
treated with reagents to test for reaction characteristics of certain ions, which may cause
color change, solid forming and other obvious visible changes. The cations to be studied
include some common alkaline earth metals, group 13 and Zn2+. These ions are not colored
in solution, and most of their compounds are white. It is impossible therefore to use colors
of solutions or precipitates to indicate which of these cations is present in solution. Instead,
in this experiment, you will use differences in solubility to separate from each other.

APPARATUS:

Small test tubes, test tube rack, litmus paper, test-tube holders, hot plate, centrifuge, three
beakers (250 mL or 400 mL), distilled water bottle, glass rod, dropping pipette, vial
containing unknown solution.
CHEMICALS:

Aqueous solutions of Ca2+, Ba2+, Mg2+, Zn2+ and Al3+

1 M Na2SO4 (aq)

6 M NaOH (aq)

6 M HCl (aq)

6 M NH3 (aq)

1 M HCl (aq)

0.25 M Ammonium oxalate, (NH4)2C204 (aq)

0.1 M NaH2PO4 (aq)

0.1 M Na2S (aq)

PROCEDURE:

Part A: Preliminary Observation

Doing the Experiment

1. 2 mL samples of 0.1 M aqueous salt of Ca2+, Ba2+, Mg2+, Zn2+ and Al3+ were placed
into small test tubes. A drop of aqueous solution was transferred to some red and
blue litmus papers with a stirring rod to test each solution to see if it is acidic, basic
or neutral. The observations were recorded in the report.

2. 1 drop of 1 M Na2SO4 (aq) was added to each test tube. The formula of the precipitate
was written in the report.

3. 1 mL of 6 M NaOH (aq) was added to each of the four remaining test tube and it was
stirred well. The formula of the products was written in the report (two precipitates
and two complex ions). The two test tubes containing complex ions were saved for
(6).

4. The two test tubes containing precipitates were centrifuged, and the solution in
each of these tubes was discarding. Each test tube was dissolved with 1/2mL 6 M
HCl (aq). If the precipitates doesnt dissolved completely, more HCl was added, a drop
at a time with stirring, until it does. Then 6 M NH3 (aq) was added, a drop at a time
until the solution is slightly basic. If a precipitate formed 1 M HCl (aq) was added
dropwise until it just dissolved. 1 drop of 0.25 M (NH4)2C204 (aq) was added to each
test tube. The formula of the precipitate was written in the report.

5. To the test tube above (4) where no precipitate formed with ammonium oxalate, 2
drops of 6 M NH3 (aq) was added and a few of 0.1 M NaH2PO4 (aq). The precipitates,
which may form slowly, had the formula MNaH2PO4, where M is the metal ion. The
formula of the precipitate was written in the report.

6. 1.5 mL of 6 M HCl (aq) was added to the two test tubes from (3) containing complex
ions. It was tested with litmus paper. If any precipitate remained, or if the solutions
are not distinct acidic, more HCl was added until any precipitate present is dissolved
and the solutions are acidic.
 Then, 6 M NH3 (aq) (at least 1 mL) was added until the solutions are distinctly basic
and have a strong odor of ammonia. It was stirred well. The formula of the
precipitates was written on the report. In the other test tube a new complex ion has
been formed. The formula was written in the report.

7. Finally, several drops of 0.1 M Na2S (aq) was added to the last test tube. The formula
of the precipitate was written in the report. The content of this test tube was
discarding in the sink under the hood. When it is in contact with acid in the drain
H2S(g) (rotten egg gas) was formed, which is not only unpleasant but poisonous.

Part B: Analysis of the Unknown.

1. The test as in Part A was carried out on unknown S4 and the cation present in each
solution was identified.

2. The observations were recorded in the table.

Questions (Part A and B)

1. Which solutions are acidic to litmus?

The solutions are acidic to litmus are Zn2+, Al3+ .

2. Which solutions are basic to litmus?

No of the solutions are basic.

3. Write the formulas of the products in the spaces provided.

Procedure (Part A) Precipitates Complex ions

2 BaSO4
3 Mg(OH)2, Ca(OH)2 Zn(OH)2, Al(OH)3
4 CaC2O4
5 Mg(H2PO4)2
6 2AlCl3 ZnCl2
7 Al2S3
4. Write the ionic equations for the ten reactions which produce the ten products
listed above.

No. Net ionic equations

1 Ba2+ + Na2SO4 2Na+ + BaSO4

2 MgSO4 + 2NaOH Mg(OH)2 + Na2SO4

3 CaSO4 + 2NaOH Ca(OH)2 + Na2SO4

4 ZnSO4 + 2NaOH Zn(OH)2 + Na2SO4

5 Al2(SO4)3 + 2NaOH 2Al(OH)3 + 3Na2SO4

6 Ca(OH)2 + (NH4)2C204 CaC204 + 2NH4OH

7 Mg(OH)2 + 2NaH2PO4 Mg(H2PO4)2 + 2NaOH

8 Zn(OH)2 + 2HCl ZnCl2 + 2H2O

9 2Al(OH)3 + 6HCl 2AlCl3 + 6H2O

10 2AlCl3 + 3Na2S Al2S3 + 6NaCl

5. Summarize your analysis in the following table:

Unknown solution Ions found

4 Al3+
 DISCUSSION:

In this experiment, the cations in known and unknown samples were identified by
using analysis technique. The cations that were been used are Ca2+, Ba2+, Mg2+, Zn2+ and Al3+.
Zn2+, Al3+ were acidic because they change the blue litmus paper to red while Ca2+, Ba2+,
Mg2+ were neutral because they do not change either the red litmus paper or the blue
litmus paper. These ions are not colored in solution, and most of their compounds are
white. Therefore, the cations were determined which are acidic, basic or neutral cations by
using litmus paper.
Then all the cations were tested with sodium sulphates, Na2SO4 (aq). MgSO4, CaSO4,
ZnSO4, and Al2(SO4)3 were all soluble, but not for the barium sulphate, BaSO4. Calcium
sulphate is slightly soluble and will not precipitate under the conditions of this
experiment. Thus, when the sulphate was added to a mixture of these cations, it was
allowed to detect the barium, Ba2+ and it could be removed from solution. After that,
another four of the sulphate cations would be tested with sodium hydroxides, NaOH (aq). The
MgSO4, CaSO4 were formed precipitate in a strongly basic solution. However, ZnSO4, and
Al2(SO4)3 are amphoteric and they dissolved in a strongly basic solution to form complex ion.
The two which precipitate can be separated due to differences in the solubility of their
oxalates. One of them would form precipitate when ammonium oxalate was added that is
Ca(OH)2 change to CaC204 . The Zn(OH)2 and Al(OH)3 solutions containing the complex ions
would then be acidified with HCl(aq), then neutralized with NH3(aq). In this weakly basic
solution, the zinc hydroxides, Zn(OH)2, would form precipitate, while the aluminium
hydroxides, Al(OH)3, solution forms a complex ion that is AlCl3. Lastly, the last cation that is
AlCl3 was precipitated with Na2S (aq) and it fomed Al2S3. The unknown S4 solution was been
identified as Al3+ because it had the similar characteristic with Al3+.

CONCLUSION:

Based on the experiment that was conducted the cations in unknown S4 solution was been
identified as Al3+.
REFERENCE:

Che Faridah Osman, Cindy Tan Soo Yun. Inorganic Chemistry Laboratory Experiments for
Inoganic Chemistry, 17th December 2013.
http://www.chemistry.sc.chula.ac.th/