UNIVERSITI TEKNOLOGI MARA,

CAWANGAN PERLIS, KAMPUS ARAU

CHM 361
EXPERIMENT 1: QUALITATIVE ANALYSIS OF CATIONS:

Ag+, Fe3, Cu2+ AND Ni2+

NAME: NURUL ASYIQIN BINTI RUSLI

STUDENT ID: 2017287454
GROUP: RAS1205C
LECTURE’S NAME: DR. SHARIZAL BIN HASAN
DATE OF EXPERIMENT: 26/9/2019
DATE OF SUBMISSION: 3/10/2019
OBJECTIVES

1. To identify the cations in known and unknown samples.

2. To construct a logical flow chart for identifying the components of a mixture of unknown
cations.

INTRODUCTION

Qualitative analysis is used to identify and separate cations and anions in a sample
substance. Unlike quantitative analysis, which seeks to determine the quantity or amount of
sample, qualitative analysis is a descriptive form of analysis. In an educational setting, the
concentrations of the ions to be identified are approximately 0.01 M in an aqueous solution.
The "semi-micro" level of qualitative analysis employs methods used to detect 1-2 mg of an
ion in 5 mL of solution.

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. The physical examination of the unknown salt involves the study of
colour, smell and density. The test is not much reliable, but certainly helpful in identifying some
coloured cations. Characteristic smell helps to identify some ions like ammonium ion.

APPARATUS

1. Small test tubes

2. Test tube rack
3. Litmus paper
4. Test-tube holder
5. Centrifuge
6. Distilled water bottle
7. Glass rod
8. Dropping pipette
9. Vial containing unknown solution

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CHEMICALS

1.
Aqueous solution of Ca2+, Ba2+, Mg2+, Zn2+, and Al3+
2. 1 M Na2SO4 (aq)
3. 6 M NaOH (aq)
4. 6 M HCL (aq)
5. 6 M NH3 (aq)
6. 1 M HCL (aq)
7. 0.25 M Ammonium oxalate, (NH4)2C2O4 (aq)
8. 0.1 M NaH2PO4 (aq)
9. 0.1 M Na2S (aq)

PROCEDURE

Part A: Preliminary Observation

Doing the Experiment

1. 2 mL of 0.1 M aqueous solutions of salt of Ca2+, Ba2+, Mg2+, Zn2+, and Al3+ (nitrates or
chlorides) was added into five small test tubes. Each solution was tested to see if it is
acidic, base or neutral by transferring a drop to some red and blue litmus papers with
a stirring rod. The observations were recorded.
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 tubes and being
stirred well. The formula of the products (two precipitates and two complex ions) was
written in the report. The two test tubes containing complex ions were saved for (6).
4. The two test tubes that containing precipitates were centrifuged and the solution in
each of these test tubes were discarded. The appearance of the two precipitates were
noticed and the solutions were dissolved with ½ mL of 6 M HCL (aq). More HCL were
added a drop at a time with stirring if the precipitate doesn’t dissolve completely. 6 M
NH3 (aq) was added a drop at a times until the solution is slightly basic. 1 M HCL (aq) was
added dropwise if a precipitate form until it dissolved. 0.25 M Ammonium oxalate,
(NH4)2C2O4 (aq) was added to each test tube. The formula of the precipitate was written
in the report.
5. 2 drops of 6 M NH3 (aq) and a few drops of 0.1 M NaH2PO4 (aq) were added to the test
tube above (4) where no precipitate formed with ammonium oxalate. The formula of
the precipitate was written in the report.
6. 1.5 mL of 6 M HCL (aq) were added to the two test tubes from (3) containing complex
ions and then were tested with litmus paper. More HCL were added if any precipitate

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 remains, or the solutions are not distinct acidic until any precipitate present is dissolved
and the solutions are acidic.
6 M NH3 (aq) was added (at least 1 mL) until the solutions are distinctly basic and have
a strong odor of ammonia. The formula of the precipitate was written in the report.
7. Several drops of 0.1 M Na2S (aq) were added to the last test tube. The formula of the
precipitate was written in the report. The content of this test tube was \ discarded in
the sink under the hood. H2S (g) was formed.

Part B: Analysis of the Unknowns

1. The test was carried out as in Part A on solution S1 and S2 and the caution that
present in each solution was identified.
2. The observations were recorded in the table.

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FLOW CHART

Ca2+, Ba2+, Mg2+, Zn2+,

and Al3+

1 drop of 1 M
Na2SO4

Ca2+, Mg2+, Zn2+, and Al3+ Ba2+ become

dissolved precipitate and
cloudy solution
1 Ml of 6 M
NaOH

Ca2+ and Mg2+ Zn2+ and Al3+ produce

become precipitate complex ions

(1) centrifuge
1.5 mL of 6 M HCL
(2) Few drops of 6M HCL and
0.25 M (NH4)2C2O4

Ca2+ form white Mg2+ dissolved Zn2+ form light Al3+ become
precipitate precipitate precipitate
2 drops of 6 M
Few drops of
NH3 and few Few drops of
0.1 M Na2S
drops of 0.1 M 0.1 M Na2S
NaH2PO4

Zn2+ became
Al3+ form
clear solution
cloudy and
thick
Mg2+ form
precipitate
precipitate

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QUESTIONS (PART A AND PART B)

1. Which solutions are acidic to litmus?

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

2. Which solutions are basic to litmus?

No of the solutions are basic.

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

Procedure Precipitates Complex Ions

(Part A)
2 BaSO4
3 Mg(OH)2 , Ca(OH)2 Zn(OH)2 , Al(OH)3
4 CaC2O4
5 Mg(H2PO4)2
6 2AlCl3 ZnCl3
7 Al2S3

4. Write the ionic equation 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 + NaSO4
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)2C2O4 CaC2O4 + 2NH4OH
7 Mg(OH)2 + 2NaH2PO4 Mg(H2PO4) + 2NaOH

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

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

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 10 2AlCl3 + 3Na2S Al2S3 + 6NaCl

5. Summarise your analysis in the following table:

Unknown Solutions Ions Found

S1 Ba2+

S2 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+.
These ions are not coloured in solution. Therefore, these cations were determined which are
acidic, basic or neutral cations by using litmus paper. Ca2+, Ba2+, Mg2+ were neutral because
they do not change either blue litmus paper or the red litmus paper while Zn2+ and Al3+ were
acidic because they change the blue litmus paper to red.

MgSO4, CaSO4, ZnSO4, and Al2(SO4)3 were all soluble when tested with sodium sulphates,
Na2SO4 but not for barium sulphate, BaSO4. Barium sulphate become precipitate and has
cloudy solution. Then, another four of the sulphate cations would be tested with sodium
hydroxides, NaOH. The MgSO4, CaSO4 were formed precipitate in a strongly basic solution.
Meanwhile, ZnSO4 and Al2(SO4)3 were dissolved in a strongly basic solution to form complex
ion. Ca(OH)2 change to CaC2O4 and form precipitate when ammonium oxalate was added.
The Zn(OH)2 and Al(OH)3 would then be acidified with HCL and then neutralized with NH3.
The Zn(OH)2 form precipitate at the bottom of the test tube while Al(OH)3 form cloudy
precipitate at the top of the solution in the test tube and forms a complex ion that is AlCl3.
Lastly, the last cation that is AlCl3 was precipitated with Na2S and it formed Al2S3. The unknown
solution was been identified as Al3+ because it has similar characteristic with Al3+.

CONCLUSION

Based on the experiment, the cation in unknown S4 solution was been identified as Al3+.

REFERENCES

https://www.thoughtco.com/qualitative-analysis-in-chemistry-608171

http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/qualitative-analysis

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https://www.scribd.com/doc/187688838/Qualitative-Analysis-of-Cations