UNIVERSITI TEKNOLOGI MARA

SARAWAK
PUSAT PENGAJIAN SAINS GUNAAN
KAMPUS SAMARAHAN 2

CHM 577

GROUP : AS222 3A

EXPERIMENT NO. : 1&2

1. QUALITATIVE ANALYSIS FOR

IDENTIFICATION OF METAL CATIONS
TITLE : 2. QUALITATIVE ANALYSIS OF
TRANSITION METAL CATIONS: Ag , Cu2+
+

and Zn2+

STUDENT’S NAME : MOHAMMAD ASHRAFF BIN SANUDDIN

STUDENT’S NO. : 2018410712

JULIA ANAK BALING
LAB PARTNERS :
DZUREEN BINTI JULAIHI
23th SEPTEMBER 2019 (EXP 1)
DATE OF EXPERIMENT :
30th SEPTEMBER 2019 (EXP 2)

DATE OF SUBMISSION : 7th OCTOBER 2019

LECTURER’S NAME : DR. YANTI YANA HALID
Objective
To perform qualitative analysis to identify metal cations.
To perform qualitative analysis to identify transition metal cations.

Introduction
There are five groups of metal cations that can be classified based on their chemical
and physical properties. The five groups are as follow:
a)
Analytical Group I Cations which are Ag+, Hg2+, Pb2+. These cations can form
precipitate when reacted with HCL.
b)
Analytical Group II Cations which are As3+, Bi3+, Cd3+, Cu2+, Hg2+, Pb2+, Sn4+ that
form precipitate when reacted with acidic H2S.
c)
Analytical Group III Cations. These metal cations can formed precipitate when
reacted with H2S in NH3. Example of cations are Co3+, Fe2+, Mn2+, Ni2+, Zn2+, Al3+ and
Cr3+.
d)
Analytical Group IV Cations like Ba2+, Ca2+, Mg2+ and Sr2+ that can form
precipitate when reacted with (NH4)2CO3 or NH4HPO4
e)
Analytical Group V Cations. Na+ and K+ give soluble salts when reacted with
(NH4)2CO3 or NH4HPO4.

Procedure Experiment 1
Procedure A
1. 2 drops of 6 M HCL was added to 1 mL of the mixture of the metal cations.
2. Precipitate (ppt.) formed and was centrifuge for 1 minute.
3. 1 additional drop of 6 M HCL was added to the clear supernatant to check for
complete precipitation.
4. The supernatant was centrifuged again fro 1 minute due to ppt. Observed.
5. The supernatant decant in a clean test tube and saved for procedure B.

Procedure B
1. 5 drops of 6 M NH3 was added to the solution to basic it.
2. The sample put in a boiling water for 3 minutes to remove excess NH3.
3. Distilled water added to the soluton up until 2 mL and 10 drops of 6M HCL was
added.
4. The sample heated in a boiling water bath for 10 minutes to produce H2S in
hydrolysis of thiocetamide.
5. Ppt. of sulfide formed, the solution was centrifuge for 2 minutes and decant to the
clean test tubes.
6. The supernatant saved for procedure C.

Procedure C
1. 3 drops of 1M thiocetamide was added to the solution and reheated for 5 minutes to
testy for complete precipitation.
2. Ppt. formed. The solution centrifuged for 2 minutes and decant the supernatant into
a clean test tube. The ppt. discarded.
3. The solution was added by distilled water until 3 mL and 10 drops of 6M HCL and
10 drops of 6M NH3 were added into the solution.
4. 5 drops of 6M NH3 was added to make the solution basic.
5. 5 additional drops of 6M NH3 and 12 drops of 1M thiocetamide were added and the
mixture stirred thoroughly.
6. The sample heated in a boiling water bath for 10 minutes.
7. Ppt. sulfide formed. The sample centrifuged and decant. The present of Zn2+ ppt. as
Zn(OH)2.
8. The supernatant save for procedure D.

Procedure D
1. 5 drops of 6M NH3 was added to the solution to make it basic.
2. 13 drops of NH3 was added to buffer the solution.
3. 25 drops of (NH4)2CO3 was added to the sample and stirred.
4. The test tube containing ppt. of carbonate was transfer to a warm water bath of
70℃ for 3 minutes. Do not boil the sample.
5. Then, the mixture was centrifuged.
*Note- there should be a ppt when added all the solution as mentioned in procedure
D, but the ppt. not formed, so the experiment ended here.*
Procedure of Experiment 2
Procedure A
1. 2 drops of 6 M HCL was added to 1 mL of the mixture of the metal cations.
2. Precipitate (ppt.) formed and was centrifuge for 1 minute.
3. 1 additional drop of 6 M HCL was added to the clear supernatant to check for
complete precipitation.
4. The supernatant was centrifuged again for 1 minute due to ppt. observed.
5. The supernatant decant in a clean test tube and saved for procedure B.
6. The ppt. Then added with 10 drops of NH3 and stirred until dissolved.
7. 5 drops of 6M HNO3 was added to the solution.
8. Ppt. formed means the presence of Ag+ was confirmed.

Procedure B
1. 5 drops of 6 M NH3 was added to the solution to basic it.
2. The sample put in a boiling water for 3 minutes to remove excess NH3.
3. Distilled water added to the soluton up until 2 mL and 10 drops of 6M HCL was
added.
4. The sample heated in a boiling water bath for 10 minutes to produce H2S in
hydrolysis of thiocetamide.
5. Ppt. of sulfide formed, the solution was centrifuge for 2 minutes and decant to the
clean test tubes.
6. The supernatant saved for procedure C.
7. The ppt. washed and centrifuged.
8. The supernatant was discard while the ppt. saved.
9. 20 drops of HNO3 was added to the ppt. and boiled for 5 minutes with stirring
occasionally.
10. Centrifuge again and the sample was decant. The ppt. was discarded.
11. 6 drops of 6M NH3 and 6 drops of 6M HNO3 were added into the supernatant.
12. 10 drops of 0.1 M K4Fe(CN)6 was added and stirred. The ppt. formed confirmed
the presence of Cu2+.
Procedure C
1. 3 drops of 1M thiocetamide was added and reheated for 5 minutes in the water bath
to test the solution for complete ppt.
2. Ppt. formed. The sample centrifuge and the supernatant was decant.
3. The solution was added with distilled water untio 3 mL and 10 drops of 6M HCl
was added.
4. 10 drops of 6M NH3 was added to buffer the solution.
5. 5 more drops of 6M NH3 was added to make the solution basic and 12 drops of 1M
thiocetamide also added.
6. The mixture stirred thoroughly and heated for 10 minutes in a boiling water bath.
7. Ppt. formed and centrifuge.
8. The solution was decant and the supernatant was discarded.
9. 1 drop of 6M NH3 was added into the ppt. and then centrifuge.
10. Supernatant discarded and the ppt. was added by 20 drops of 6M HNO3.
11. The mixture was heated in a boiling water bath for 5 minutes with stirring and
then centrifuge.
12. The mixture decant and the supernatant was added with 5 drops of 6M NH3 to
make it basic.
13. 5 drops of 6M CH3COOH and 10 drops of K4Fe(CN)6 were added.
14. Ppt. formed and was centrifuge. The ppt. confirmed the presence of Zn2+.

Result of Experiment 1
1. On adding HCL to the initial sample
Solution Observation Balanced chemical equation
Unknown White precipitate Ag+ + Cl- → AgCl (aq)

2. On adding H2S under acidic solution

Solution Observation Balanced chemical equation
Unknown Black precipitate Cu2+ + S2- → CuS (aq)
3. On adding H2S under basic solution
Solution Observation Balanced chemical equation
Unknown White precipitate Zn2+ + 2NH3 + 2H2O → Zn(OH)2 +
2NH4

4. On adding CO32-
Solution Observation Balanced chemical equation
Unknown No observable changes -

Unknown number 2 contains Ag+ and Cu2+ ions.

Result of Experiment 2
1. On adding HCL to the initial sample
Solution Observation Balanced chemical equation
Unknown White precipitate Ag+ + Cl- → AgCl (aq)
Confirmatory test for the cation
Unknown White precipitate Ag+ + Cl- → AgCl (aq)

2. On adding H2S under acidic solution

Solution Observation Balanced chemical equation
Unknown Black precipitate Cu2+ + S2- → CuS (aq)
Confirmatory test for the cation
Unknown Brown precipitate 2Cu2+ + Fe(CN)64- → Cu2[Fe(CN)6] (s)

3. On adding H2S under basic solution

Solution Observation Balanced chemical equation
Unknown Dark green Zn2+ + S2- → ZnS (aq)
precipitate
Confirmatory test for the cation
Unknown Brown precipitate 2Cu2+ + Fe(CN)64- → Cu2[Fe(CN)6] (s)

Unknown number 2 contains Ag+ and Cu2+ ions.

Discussion
In this experiment, the precipitate formed after added precipitate reagent gave the
positive reaction of the metal cation except in procedure D in experiment 1 where
there is no precipitate after the solution centrifuge.
For the procedure A , the HCl used to detect the presence of Ag+ ions. This
proved when there is formation of white precipitate that indicates the present of Ag+
ions. The unknown 1 for both experiment gave the positive result. The balanced
chemical equation shown below:
Ag+ (aq) + Cl- (aq) → AgCl (aq)

Presence of Cu2+ were done in unknown 2 for experiment 1 and mixture of

experiment 2 after H2S added in acidic condition where black precipitate can be
observed. The balanced chemical equation for the reaction as follow:
Cu2+ (aq) + S2- (aq) → CuS (aq)

The precipitated was tested with 0.1 M K4Fe(CN)6 to prove the Cu2+ ion in the
solution. The brown precipitate prove that they contain Cu2+ ion.
2Cu2+ + Fe(CN)64- → Cu2[Fe(CN)6] (s)
Grey precipitate should form after the addition of H2S in basic condition that
show the present of Zn2+ ion. But there is an error in both experiment, where in
experiment 1, white precipitate formed. Whereas in experiment 2, dark green
precipitate formed. The incomplete reaction could happen due to the wall of the tube
was contaminated by other chemicals. Therefore, confirmatory test is needed to prove
the present of Zn2+ ion. 10 drops of K4Fe(CN)6 was added in the last step and brown
precipitate formed indicate that there is Zn2+ ion.
2Cu2+ + Fe(CN)64- → Cu2[Fe(CN)6] (s)
There is an error in experiment 1 where the procedure cannot be done further
(procedure D(i) and (ii)) due to the precipitate not formed even though already been
centrifuge. The experiment stop at procedure D and can’t be proceed. This might be
the incomplete reaction due to contaminate from other chemical.
Conclusion
Precipitate method is one way of qualitative analysis to identify the ion present in
metal cations or in transition metal cations. The precipitation gave various in colour
especially for metal transition because it have more than one oxidation number. In
experiment 1, the mixture solution contained Ag+, Cu2+, Zn2+ and K+ ions. Meanwhile,
the mixture solution in experiment 2 contained Ag+, Cu2+ and Zn2+ ions. All of these
ions presence are been tested for confirmatory except for K+ ion due to some error
when conducting the experiment.

References
Lab Report Qualitative Analysis for Identification of Metal Ions at
http://www.bartleby.com/essay/lab-report-qualitative-analysis-for-identification-of-P
KJV2LEKVC
Qualitative Analysis Tests for Metal Cations Identifying Positive Ions at
http://www.docbrown.info/page13/ChemicalTestsc.html
Qualitative Analysis- Wired Chemist at
http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/qualitative-
analysis