UNIVERSITI TEKNOLOGI MARA (PERLIS)

Chm 475 : LAB REPORT

STUDENT NAME : ROHAYA BINTI MOHMAD SUBOH

2015249872

EXPERIMENT :3

TITLE : QUALITATIVE ANALYSIS OF

TRANSITION METAL CATIONS

(Ag2+, Zn2+, Cu2+ )

LAB GROUP : RAS2452b

DATE OF REPORT SUBMISSION : 15 October 2015

LAB PARTNER’S NAME : MUHAMMAD LUQMAN BIN ALI

LECTURER’S NAME: SIR SHUKRI ISMAIL

INTRODUCTION

Based on their chemical and physical behavior, analytically, metal cations can be classified into five
groups as listed below:

a) Analytical Group I Cations

Ag+ , Hg2+ , Pb2+
Form precipitate when reacted with HCl

b) Analytical Group II Cations

As3+ , Bi3+ , Cd3+ , Cu2+, Hg2+ , Pb2+ , Sn4+
Form precipitate when reacted with acidic H2S

c) Analytical Group III Cations

Co3+ , Fe2+ , Mn2+ , Ni2+ , Zn2+ , *Al3+ , Cr3+
Form precipitate when reacted with H2S in NH3
*Al3+ is separated as Al(OH)3

d) Analytical Group IV Cations

Ba2+ , Ca2+ , Mg2+ , Sr2+
Form precipitate when reacted with (NH4)2CO3 or NH4HPO4

e) Analytical Group V Cations

Na+ , K+
Form soluble salts when reacted with (NH4)2CO3 or NH4HPO4

In this experiment, we will conduct some test on confirmation on the presence of Ag+, Cu2+ and Zn2+
only. The confirmation test usually using redissolving the metal cation then followed by reprecipating
it by involves the complex ions which is confirming reagent for that particular cation.

OBJECTIVE

The objective of the experiment is to perform qualitative analysis to identify transition metal cations.

PROCEDURE

Procedure A

Two drops of 6M HCl is added into 1 mL of the solution which is mixture of metal cations (
Zn2+, Cu2+, Ag+ ) .If precipitate of chloride is formed, the suspension is centrifuge for 1 minute.
One additional drop of 6M HCl is added to the clear supernatant to check for complete
precipitation. If precipitate is observed in the supernatant, centrifuge again for 1 minute.
Decant the supernatant in a clean test tube. The supernatant is saved for further tests.
Confirmation test for presence of Ag+

The precipitate from procedure A is wash with 2 mL of distilled water by centrifuge it. Then
10 drops of 6 M NH3 and stir to dissolve the solution. If there is color changes, add 6 M HNO3
solution dropwise until the precipitate is formed.

Procedure B

Next, to the supernatant from procedure A, 6M NH3 is added dropwise to the solution until it
is basic. The sample is put in a boiling water bath for 2-3 minutes to remove excess NH3. The
volume of the solution is adjusted to 2 mL with distilled water and added 10 drops of 6M HCl.
12 drops of thioacetamide is added to the solution and stirred. The sample is heated in boiling
water bath for 10 minutes to allow for the hydrolysis of thioacetamide producing H 2S. If
precipitate of sulfide is formed, centrifuge for 2 minutes, decant the supernatant to a clean
test tube. The supernatant is saved for further tests.

Confirmation of Cu2+

The precipitate from procedure B is wash with 2 mL of distilled water and centrifuge. The
precipitate is save while discard the supernatant. Then, 20 drops of 6M HNO3 is added to the
precipitate. The sample is boiled for several minutes with stirring occasionally in boiling water bath. If
black precipitate is formed, centrifuge the solution. Next, save the supernatant for futher test and
discard the precipitate. To the supernatant, add dropwise oof 6M NH3 until the solution is basic.
Continued to add 6M HNO3 until the solution is acidic. Then, add 10 drops of 0.1 M K4Fe(CN)6 and stir
until red maroon precipitate is formed.

Confirmation of Zn2+

The supernatant from procedure B is added with 3 more drops of 1M thioacetamide to test
for complete precipitation and reheat for 5 more minutes in the water bath. If there is precipitate
formed, centrifuge the sample. The supernatant is save for further test while discard the precipitate.
The volume of supernatant is adjusted until 3 ml with the distilled water. Next add 10 drops of 6M
HCl, add more 10 drops of 6M NH3 to buffer then add dropwise of 6 M NH3 until the solution is basic.
Add 5 more drops of NH3. 12 drops of 1M thioacetamide is added and stir thoroughly and heat the
solution for 10 minutes in a boiling water bath. If precipitate is formed, centrifuge the solution. The
supernatant is discard and the precipitate is wash with 2 mL of distilled water. Centrifuge the solution
and discard the supernatant. Add 1 drop of 6 M NH3 into the precipitate and centrifuge again. The
supernatant is discard and 20 drops of 6 M HO3 is added to the precipitate. Then heat the sample in
boiling water bath for several minutes with stirring. Centrifuge and discard the precipitate and used
the supernatant for confirmation test. To the supernatant, 6 M NH3 is added until basic then added
drops of 6 M CH3COOH until acidic. Lastly add 10 drops of of 0.1 M K4Fe(CN)6 and stir until grey
precipitate is formed.
RESULT AND DISCUSSION

No Test result conclusion

Adding HCl to the initial Known: White precipitate formed Known :There is presence of
sample for known and Group I cations
1 unknown solution Unknown : no precipitate is formed
Unknown : No presence of
No color changes Group I cations

Confirmation test for cation Known : white precipitate is formed Known : Ag+ is presence

Unknown : no precipitate formed Unknown : No presence of

Ag+

Adding H2S under acidic Known: Black precipitate formed Known :There is presence of
condition for known and Group II cations
2 unknown solution Colorless solution turn to black
Unknown : There is
Unknown : Black precipitate is formed presence of Group II cations
Colorless solution turn to black

Confirmation test for cation
Known : Red- maroon precipitate is Known : Cu2+ is presence
formed
Unknown : Cu2+ is presence
Unknown : Red-maroon precipitate
formed

Adding H2S under basic Known: White precipitate formed Known :There is presence of
solution Group III cations
3
Unknown : presence of
Unknown : White precipitate is formed
Group III cations

Confirmation test for cation Known : Lime precipitate is formed Known : Zn2+ is is presence

Unknown : Lime precipitate formed Unknown : presence of Zn2+

Based on this experiment, there are two result is obtained which is known solution and unknown
solution. In the known solution, we can conclude that the mixture solution contained of Ag+, Cu2+ and
Zn2+ . This is because of when added the HCl solution to initial sample, white precipitate is formed.
After conduct the confirmation test for the cation , white precipitate is formed that shown the
presence of Ag+. Then after continued with adding H2S under acidic condition, black precipitate is
formed and red- maroon precipitate is form when conduct the confirmation test for Cu2+ . This prove
the presence of Cu2+. Next, after adding H2S under basic solution, white precipitate is formed and after
being tested, there is lime precipitate formed. It shown there is presence of Zn2+.

For the unknown mixture, we are using the unknown number 2. When being adding with HCl solution
to initial sample, no precipitate is formed. This shown there is no presence of Ag+. Then, we continued
with adding H2S under acidic condition, black precipitate is formed and red- maroon precipitate is form
when we done the confirmation test for Cu2+ . This prove the presence of Cu2+. Next, after adding H2S
under basic solution, white precipitate is formed and after being tested, there is lime precipitate
formed. It shown there is presence of Zn2+. So we can conclude that there are presence of Cu2+ and
Zn2+ in the solution.

CONCLUSION

In conclusion, the objective of this experiment is determined. The presence of Ag+ , Cu2+ and Zn2+ is
being confirmed. In the unknown solution, only Cu2+ and Zn2+ are present.

REFERENCE

Retrieved from http://geo1.tcu.edu/richards/Lab%209.pdf