EXPERIMENT 1

QUALITATIVE ANALYSIS FOR IDENTIFICATION OF METAL CATIONS

&
EXPERIMENT 2
QUALITATIVE ANALYSIS OF TRANSITION METAL CATIONS: AG⁺, CU²⁺ AND ZN²⁺

COURSE CODE: ED 475

NAME: NORHAFIZA BINTI SAMSUDIN
LAB PARTNER: SITI HAZIRAH BINTI ZUBARI
INTRODUCTION

Qualitative analysis is a process to identify the chemical properties of an unknown substance.

This separation method are usually used to classify substances. The reagent are added to the
solution mixture and cause precipitation to form. Example of reagent that been used like
ammonia (NH₃) and many more. For example reaction, between copper and sulphur, where
light blue precipitate is formed. The chemical equation of this reaction:

Cu²⁺ (aq) + S²ˉ (aq) → CuS (s)

There is special exception of the solubility of ion. Transition element will form many colour
of precipitate. This is happen because of it depends on how many number of oxidation of the
element. This experiment identify the presence of ion based on the precipitation. Metal
cations can be classified into five groups which is group 1 is Ag⁺, Hg²⁺, Pb²⁺ that will form
precipitate when react with HCl. Group 2 is As³⁺, Bi³⁺, Cd³⁺, Cu²⁺, Hg²⁺, Pb²⁺,Sn⁴⁺ will form
precipitate when react with H₂S. Group 3 is CO³⁺, Fe²⁺, Mn²⁺, Ni²⁺, Zn²⁺, *Al³⁺, Cr³⁺ will form
precipitate when react with H₂S in NH₃ (*Al³⁺ will separate as Al(OH)₃). For group 4 is Ba²⁺,
Ca²⁺, Mg²⁺, Sr²⁺ will form precipitate if react with ammonium carbonate or ammonium
phosphate. Lastly, group 5 is Na⁺ and K⁺ will form soluble salt when react with ammonium
carbonate or ammonium phosphate.

OBJECTIVE

To determine the metal cations in the mixture of solution.

APPARATUS AND EQUIPMENT

Test tube, centrifuge, test tube rack, glass rod, measuring cylinder, litmus paper, test tube
holder, distilled water, water bath, 6M of HCl, 6M NH₃, 1M thioacetamide, 6M acetic acid
and 1M K₂CrO₄, unknown 1, unknown 2 and mixture of solution.
METHOD

EXPERIMENT 1:
 Figure 1 show the flowchart of the identification of metal cations in Experiment 1.

Experiment 2:
Figure 2
 Figure 2.1
Figure 2 and 2.1 showed the steps and the colour changed of transition metal cations.

DATA
Experiment 1: Qualitative analysis for identification of metal cations.

1) On adding HCl to the initial sample

Solution Observation Balanced chemical equation

Unknown 1 White ppt is formed Ag⁺(aq) + Clˉ(aq) → AgCl

Unknown 2 No ppt is formed No reaction

Mixture White ppt is formed Ag⁺(aq) + Clˉ(aq) → AgCl(s)

2) On adding H₂S under acidic condition
Solution Observation Balanced chemical equation

Unknown 1 No ppt is formed No reaction

Unknown 2 White ppt is formed Pb²⁺(aq) + S²ˉ(aq) → PbS(s)

Mixture Light blue ppt is formed Cu²⁺(aq) + S²ˉ(aq) → CuS(s)

3) On adding H₂S under basic condition

Solution Observation Balanced chemical equation
Unknown 1 Grey ppt is formed Zn²⁺(aq) + 2OHˉ(aq) →
Zn(OH)₂(s)
Unknown 2 Grey ppt is formed Zn²⁺(aq) + 2OHˉ(aq) →
Zn(OH)₂(s)
Mixture Grey ppt is formed Zn²⁺(aq) + 2OHˉ(aq) →
Zn(OH)₂(s)

4) On adding CO²ˉ₃
Solution Observation Balanced chemical equation
Unknown 1 Grey ppt is formed Ba²⁺(aq) + CO²ˉ₃(aq) →
BaCO₃(s)
Unknown 2 White ppt is formed Mg²⁺(aq) + CO²ˉ₃(aq) →
MgCO₃(s)
Mixture No ppt is formed No reaction

5) On adding CrO²ˉ₄
Solution Observation Balanced chemical equation
Unknown 1 Yellow ppt is formed Ba²⁺(aq) + CrO²ˉ₄(aq) →
BaCrO₄(s)
Unknown 2 No ppt is formed No reaction
Mixture No ppt is formed No reaction
 6) On adding C₂O²ˉ₄
Solution Observation Balanced chemical equation
Unknown 1 No ppt is formed No reaction
Unknown 2 No ppt is formed Mg²⁺(aq) + C₂O²ˉ₄(aq) →
MgCO₄(s)
Mixture No ppt is formed No reaction

Unknown I contains Ag⁺ ion, Zn²⁺ ion, Ba²⁺ ion

Unknown II contains Zn²⁺ ion, Mg²⁺ ion
Mixture contains Ag⁺ ion, Cu²⁺ion, Zn²⁺ ion and K⁺ ion.

Experiment 2: Qualitative analysis of transition metal cations (Ag⁺, Cu²⁺ and Zn²⁺)

1) On adding HCl to the initial sample

Solution observation Balanced chemical equation

Unknown No ppt is formed No reaction

Mixture White ppt is formed Ag⁺(aq) + Clˉ(aq) → AgCl

Confirmatory test for the cation

Solution Observation Balanced chemical equation

Unknown No ppt is formed No reaction

Mixture White ppt is formed Ag⁺(aq) + Clˉ(aq) → AgCl

2) On adding H₂S under acidic condition

Solution Observation Balanced chemical equation
Unknown No ppt is formed No reaction
Mixture Light blue ppt is formed Cu²⁺(aq) + S²ˉ(aq) → CuS
Confirmatory test for the cation
Solution Observation Balanced chemical equation
Unknown No ppt is formed No reaction
Mixture Brick-red ppt is formed Cu²⁺(aq) + Fe(CN)⁴ˉ₆(aq) →
Cu₂(Fe(CN)₆)(s)

3) On adding H₂S under basic conditions

Solutions Observation Balanced chemical equation
Unknown Dark-greenish ppt is formed Zn²⁺(aq) + S²ˉ(aq) → ZnS(s)
Mixture White precipitate formed Zn²⁺(aq) + S²ˉ(aq) → ZnS(s)

Confirmatory test for the cation

Solutions Observation Balanced chemical equation
Unknown Yellow ppt is formed 3Zn²⁺(aq) + 2Fe(CN)⁴ˉ₆(aq) →
Zn₃(Fe(CN))₂(s)

Mixture Brick-red ppt is formed 3Zn²⁺(aq) + 2Fe(CN)⁴ˉ₆(aq) →

Zn₃(Fe(CN))₂(s)

The mixture solution contains: Ag⁺ ion, Cu²⁺ ion and Zn²⁺ ion.
The unknown solution contains: Zn²⁺ ions.

DISCUSSION
As we can discuss in this experiment, precipitation is formed when reagent is added to
the solution and give reaction that showed the metal cation. But, there is also no precipitation
is formed when reagent is added which is the product is invisible.

Test 1 is HCl is used to detect the presence of Ag⁺ ion. White precipitation that
formed at the bottom of test tube shows that Ag⁺ ions is presence. 10 drops of 6M NH₃ is
added to make confirmatory test and to dissolve the precipitation that presence. 6M HNO₃ is
added and formed white precipitate again. The unknown 1 and mixture solution for both
shows a positive result. The balanced equation is:

Ag⁺(aq) + Clˉ(aq) → AgCl

In test tube unknown 2 and mixture in experiment 1 and mixture in experiment 2 formed a
precipitation after H₂S is added in acidic solution that indicate the presence of Cu²⁺ ion. It
should be formed black colour precipitate but due to incomplete reaction of these ion.

Cu²⁺(aq) + S²ˉ(aq) → CuS(s)

To identify Cu²⁺ ion in the solution, 0.1M K₄Fe(CN)₆ is added. After wash CuS, 6M HNO₃ is
added. 6M NH₃ is added into supernatant until it become acidic. Then, 10 drops of 0.1M
K₄Fe(CN)₆ is added and formed brick-red colour precipitation that contain Cu²⁺ ion.

To know the presence of Zn²⁺ ion, H₂S is added and formed grey precipitation. But
due to error, bright-blue precipitation is formed. 10 drops of 0.1M K₄Fe(CN)₆ is added to
form brick-red precipitate to indicate the presence of Zn²⁺. The balanced equation is:

3Zn²⁺(aq) + 2Fe(CN)⁴ˉ₆(aq) → Zn₃(Fe(CN))₂(s)

In order to detect cation group 4 and 5, supernatant is reacted with (NH₄)₂CO₃. The CO₃²ˉ ion
will produce soluble and insoluble salt. Unknown 1 formed grey precipitation and unknown 2
formed white precipitate. The precipitate will be either Ba²⁺, Ca²⁺, Mg²⁺ and Sr²⁺ ion. To
know the unknown 1 and unknown 2, 6 drops of 1M K₂CrO₄ is added and the precipitate that
formed will indicate Ba²⁺ ion. Yellow precipitate will formed from the reaction between Ba²⁺
ion and CrO₄²ˉ and become BaCrO₄. The balanced chemical equation is:

Ba²⁺(aq) + CrO²ˉ₄(aq) → BaCrO₄(s)

Meanwhile, unknown 2 does not have any reaction and need to be identify. Addition of 1M
K₂C₂O₄ to the solution and stir well. When there is no precipitate it is indicate as Mg²⁺ ion.
The balanced chemical equation is:

Mg²⁺(aq) + C₂O²ˉ₄(aq) → MgCO₄(s)

To reduce error, the equipment must be cleaned wisely by using distilled water before started.
To handle chemical substances, safety gloves must be used as we use HCl is a strong acid.
Excess chemical should be discard properly.
CONCLUSION

To sum up this experiment, qualitative analysis is one of the precipitation method to

indicate the present of ion in the solution. The transition element have various colour from
precipitation of salt because of the differences oxidation number. From the experiment 1, we
can see the presence of ion in unknown 1 are Ag⁺ ion, Zn²⁺ ion and Ba⁺ ion. In the unknown 2
have the presence of Zn²⁺ ion and Mg²⁺. The mixture solution consist of Ag⁺ ion, Cu²⁺ ion,
Zn²⁺ ion and K⁺ ion. While, in experiment 2, we can see the unknown is Zn²⁺ ion. On the
other hand, the mixture solution contain of Ag⁺ ion, Cu²⁺ ion and Zn²⁺ ion.

REFERENCES
1. Raymond Chang (2010). Chemistry (10th edition). New York McGraw Hill.
2. Silberberg, M. (2015) .The Molecular Nature of Matter and Change (7thed). New
York. McGraw Hill.