Name:______________________ PharmChem-1 Lab Date Submitted:___________________

Course/Sec:__________________(Inorganic Medicinal) Date Performed: __________________

Experiment #-02
ANALYSIS OF GROUP – II CATIONS

I. DISCUSSION:

The Group II Cations can be precipitated as sulfide of cupric, mercuric, lead, bismuth,
cadmium, arsenic, antimony, and tin ions. The Precipitating agent for the group, cations can be
H₂S or thioacetamide.

The three (3) Major Steps involved in the analysis of Group II Cations are as follows:

1. Precipitation of the groups as sulfides. Then, the subgroups are subdivided by the action of
KOH solution.

2. Analysis of Group II-A Cations.

3. Analysis of Group II-B Cations.

II. A. Chemical Reagents: Test Solutions:

3F HCl; 2F HNO₃; Conc. NH₃; Thioacetamide Solution; sat. NH₄Cl
3F KOH ; 1F K₂CrO₄; Conc. HNO₃; Ferrocyanide; sat. NH₄Ac
1F KCN; HgCl₂ Sol’n. Conc. H₂SO₄; Magnesium Ribbon SnCl₂;
3F NH₃ Conc. HCl

II. B. Laboratory Materials:

12-Test Tubes; Test-Tube Rack; Beaker; Wire Gauze; Centrifuge Machine
Bunsen Burner; Micropipette Tripod; Water Bath; Graduated Cylinder;
Evaporating Dish

III. Procedures:

A. Precipitation of Group II Cations:

1. To 1 mL of the Test Solution, add 2 drops of 2F HNO3. Heat in a water bath for 3
Minutes.
2. Make the solution barely alkaline with 3F NH₃. Then add 3F HCl until it is just acid.

3. Heat on a water bath to concentrate the solution to a volume of 1 mL. Then add 2
drops of conc. HCl
 4. Add 5 drops of thioacetamide solution. Heat in a boiling water bath for 5 minutes.

5. Add 2 mL of H₂O and 5 additional drops of the thioacetamide solution.

6. Heat again in a boiling water bath for 5 minutes.

7. Centrifuge and remove the Centrifugate. (DISCARD).

8. Wash the sulfide precipitate with 10-drops of water containing 1-drop of

thioacetamide solution. Then, add 1 drop of saturated NH₄Cl. Centrifuge. Discard the
wash H₂O. Or centrifugate when no precipitate is present/formed.

B. Separation and Identification of Group II-A Cations.

9. Wash the precipitate with 10-drops of water to remove the excess KOH. Discard
Washings.

10. Add 10 drops of 3F HNO₃. Then, heat in a water bath for 3 minutes. Centrifuge.
Analyze. the residue according to Procedure C-11. Save the centrifugate for procedure C 14.
Repeat the given procedures if much residue is left. If the residue is black, the presence of HgS
is indicated; whereas, white residue indicates Hg(NO₃)₂.2HgS and S.

C. Confirmatory Test.

C₁. For Hg⁺².

11. Dissolve the residue in 4 drops Aqua Regia (3 parts of HCl and 1 part of Conc. HNO₃).

12. Add 2 drops of H₂O and boil in a water bath for 2 minutes.

13. Cool and add 2 drops of SnCl₂ solution.

Positive Result:

White Precipitate of Hg₂Cl₂ or gray precipitate of Hg and Hg₂Cl₂ confirms

the presence of MERCURIC ion.

Chemical Reaction involved:

2HgCl₄ + SnCl₄ ====== Hg₂Cl₂ + SnCl₆ + 4Cl⁻

 14. To the centrifugate (from Procedure B-10) which contains Pb, Bi, Cu, and Cd ions,
transfer to an evaporating dish. Add 3-drops of conc. H₂SO₄. Evaporate until dense white fumes
appear and only 2 or 3 drops of the liquid remain.

15. Cool thoroughly and add 1 mL of H₂O carefully.

16. Stir thoroughly and transfer to a centrifuge tube.

17. Rinse the evaporating dish with 5 drops of H₂O and add washings to the solution.
Centrifuge.

18. Separate the precipitate from the centrifugate. Anlayze the precipitate according to
Procedure C-19.

C₂.For Pb⁺².

19. Wash the precipitate with 4-drops of H₂O and discard washing.

20. Add 10-drops of saturated NH₄Ac. Heat for 3 minutes with stirring in a water bath.

21. If the resulting solution is not clear, centrifuge and discard the centrifugate.

22. Add 1 drop of conc. HAc and 2 drops of 1F K₂CrO₄.

Positive Result:

Yellow precipitate confirms the presence of LEAD ion.

Chemical Reaction Involved:

Pb (C₂H₃O₂)₂ + CrO₄ ===== PbCrO₄ + 2C₂H₃O₂⁻

CONCLUSION/S: