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EXPERIMENT 2 : QUALITATIVE ANALYSIS OF

TRANSITION METAL IONS Ag+, Cu2+, Zn2+


NAME: NURUL FATIN BINTI RAZAK
STUDENT ID: 2014983737
CLASS: AS2452D
COURSE: CHM 431
INORGANIC CHEMISTRY
LECTURERS NAME: DR. AMALINA MOHD
TAJUDDIN

INTRODUCTION:
Transition metal also is an metal cation which is inorganic compound but there can have more
than one oxidation number. In this experiment, transition metal is confirmed by addition
process and formed coloured precipitate just like metal cation. The presence of transition
metal in mixture solution is confirmed through specific procedure. Ag2+ , Cu2+ and Zn2+ are
three transition element that will be identified in this experiment. Centrifuge is used to
separate the two immisible solution so that precipitate and supernatant can be decanted.

OBJECTIVE:
The objective of this experiment is to perform the qualitative analysis to identify the transition
metal ions in the solution.

APPARATUS AND EQUIPMENT


Test tubes, red and blue litmus paper, dropper, measuring cylinder, centrifuge, stirrer, test tube
rack, water bath.

METHOD:
Procedure A:
1. 2 drops of 6 M HCl is added to 1 mL of the mixture.
2. Precipitate is formed; the suspension is centrifuged for one minute.
3. 1 additional drop of 6 M HCl is added to the clear supernatant to
check for complete precipitation.
4. Precipitate is observed in the supernatant, the suspension is
centrifuge again for 1 minute.
5. The supernatant is decanted in a clean test tube and saved for
procedure B.
Confirmation Test of Ag+:
1. The precipitate is washed with 10 drops of 6 M NH3 and stirred until
dissolved.
2. 6 M HNO3 is added drop wise until white precipitate is formed.
Procedure B:
1. 6 M NH3 is added drop wise to the solution from A until basic.
2. The sample is put in a boiling water bath for 2-3 minutes to remove
NH3.
3. The volume of the solution is adjusted to 2 mL with distilled water
and 10 drops of 6 M HCl is added.
4. 12 drops of thioacetamide is added to the solution and stirred.
5. The sample is heated in boiling water bath for 10 minutes to allow
the hydrolysis of thioacetamide producing H2S.
6. Precipitate of sulfide is formed, the suspension is centrifuge for 2
minutes, and the supernatant is decanted to a clean test tube. The
supernatant is saved for procedure C.
Confirmation Test of Cu2+:
1. The precipitate is washed and the supernatant is discarded.
2. 20 drops of 6 M HNO3 is added and stirred for several minute.
3. The suspension is centrifuge, precipitate formed is discarded. 6 M
NH3 is added drop wise to the supernatant until basic.
4. 6m HNO3 is added drop wise until acidic and 10 drops of 0.1 M
K4Fe(CN)6 is added. The solution is stirred.

Procedure C:
1. 2 drops of 1M thioacetamide is added to the solution from B. The
solution is heated for 5 minutes to test for complete precipitation.
2. Precipitate is formed, the supernatant is centrifuge and decanted
into a clean test tube and the precipitate is discarded.
3. The volume is adjusted to 3 mL with distilled water and 10 drops of 6
M HCl and 10 drops of 6 M NH3 is added for buffer.
4. 6 M NH3 is added drop wise until the solution is basic.
5. 5 additional drops of 6 M NH3 and 12 drops of thioacetamide are
added and stirred the mixture thoroughly.
6. The sample is heated in boiling water bath for 10 minutes.
7. Precipitate of sulfide is formed, centrifuge and the supernatant is
decanted.
8. The precipitate is washed with 1 drop of 6 M NH3. Precipitate formed,
centrifuge and the supernatant is discarded.
Confirmation Test of Zn2+:
1. 20 drops of 6 M HNO3 is added and boiled in boiling water bath for
several minute with stirring.
2. The mixture is centrifuge, the supernatant is decanted into a clean
test tube while the precipitate is discarded.
3. 6 M NH3 is added drop wise to the supernatant until basic.
4. 6 M CH3COOH is added drop wise to the supernatant until acidic.
5. 10 drops of 0.1 M K4Fe(CN)6 is added. The solution is stirred.
Centrifuge the precipitate and supernatant.

RESULT AND ANALYSIS:


A. On adding HCl to the initial sample

Observation

Balanced chemical equation

Known

White precipitate formed

Ag+ + HCl AgCl(s)+ HCl

Unknown

No precipitate formed

Confirmatory test for Ag+ cation


Observation

Balanced chemical equation

Known

White precipitate formed

Ag+ + HCl AgCl(s)+ HCl

Unknown

B. On adding H2S under Acidic Condition


Known

Observation
_Solution turned blue_

Balanced chemical equation


_

Unknown

No precipitate formed

Confirmatory test for Cu2+ cation


Observation
Known

No precipitate formed

Unknown

No precipitate formed

Balanced chemical equation


_
Zn2+ + H2S ZnS + H2

C. On adding H2S under basic conditions


Observation

Balanced chemical equation

Known

No precipitate formed

Unknown

White precipitate formed

_
Zn2+ + H2S ZnS + H2

Confirmatory test for Zn2+ cation


Observation
Known

No precipitate formed

Unknown

White precipitate formed

Balanced chemical equation


_
Zn2+ + H2S ZnS + H2

The Unknown contains Ag+ , Zn2+ .

DISCUSSION:

Based on the experiment, transition metal cation of Ag+, Cu2+, Zn2+ is identified.
The experiment is started with the reaction of mixture solution by adding the hydrochloric
solution. As the hydrochloric solution is added, white precipitate is formed. Both of mixture
contain the presence of Ag+. T he result is being confirmed by adding of ammoni and nitric
acid to the precipitate. The balance chemical equation of Ag+ is :
Ag+ + HCl AgCl(s) + HCl
The experiment is continued by tested the two mixture with thioacetamide under the acidic
condition. Based on the result, both of the mixture showed negative result even though the
known mixture should have contain Cu2+. As the second experiment is failed, the experiment
is continued to identified the presence of Zn2+. Only unknown mixture showed the presence of
the transition metal cation. White precipitate is formed so that it is proved the unknown
contain Zn2+. The balanced chemical equition is written:
Zn2+ + H2S ZnS + H2
Based on the experiment, inaccuracies might happen especially regarding the known mixture.
The mixture is failed to prove that there are the presence of Zn2+ and Cu2+. These may be
caused of the supernatant were not decanted properly from the previous analysis and the
apparatus and equipment that is used are contaminated with other impurities. Other than that,
the time for observation was limited so that the precipitation process cannot be done properly.
Last but not least, the mixture were diluted too much during the preparation stage.

CONCLUSION:
In conclusion, transition metal cation in two different mixture is identified.
The unknown mixture contain Ag+ and Zn2+.

REFERENCES:

1. Classification of the Cations and Anions, P.1-17.


http://www.inc.bme.hu/en/subjects/inchem/sillabus/129-145.pdf
2. Qualitative Analysis of Cations, P.1-17, University of Leftbridge
http://classes.uleth.ca/200801/chem20001/1237%20Expt1_Qual2008.pdf