UNIVERSIDAD DE ZAMBOANGA

School of Allied Medicine (SAM)

Pharmacy Department
PHARM CHEM 1 LABORATORY
Qualitative Analysis

Name: ___________________ Course/Sec: ___________ Date Submitted: ___________________

Group Name: ______________ Schedule: _____________ 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 HS 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 HNO; Conc. NH; Thioacetamide Solution; sat. NHCl
3F KOH ; 1F KCrO; Conc. HNO; Ferrocyanide; sat. NHAc
1F KCN; HgCl Soln. Conc. HSO; Magnesium Ribbon SnCl;
3F NH 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 NH. 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 HO 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 NHCl. Centrifuge. Discard the wash HO. 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 HNO. 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(NO).2HgS and S.
 C. Confirmatory Test.

C. For Hg.

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

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

13. Cool and add 2 drops of SnCl solution.

Positive Result:

White Precipitate of HgCl or gray precipitate of Hg and HgCl confirms the presence of
MERCURIC ion.

Chemical Reaction involved:

2HgCl + SnCl HgCl + SnCl + 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. HSO. Evaporate until dense white fumes appear and only
2 or 3 drops of the liquid remain.

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

16. Stir thoroughly and transfer to a centrifuge tube.

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

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

C.For Pb.

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

20. Add 10-drops of saturated NHAc. 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 KCrO.

Positive Result:

Yellow precipitate confirms the presence of LEAD ion.

Chemical Reaction Involved:

Pb (CHO) + CrO PbCrO + 2CHO

CONCLUSION/S: