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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 #-01
ANALYSIS OF GROUP I CATIONS

I. DISCUSSION:

The Group I Cations are those that form precipitates when they combine with chlorides.
These chlorides that are insoluble in dilute acids are Silver chloride, Mercurous chloride, and
Lead chloride. The solubility values of the given chlorides are as follows: PbCl=0.04F
(approximately); HgCl=7.5x10 F, and AgCl=1.3x10 F. The given values indicate that the
precipitation of AgCl and HgCl are almost complete, whereas the precipitation of PbCl is
always incomplete and there can be no precipitation at low concentration. PbCl can be
separated from AgCl and HgCl by treating the solution with Hot Water. The solubility of PbCl
increases by 5 times as the temperature is increased. AgCl is separated from HgCl by its
solubility in NH to form Ag(NH).

The three (3) Principal Steps involved in the analysis of Group I Cations are as follows:
1. The group is precipitated with dilute HCl as insoluble chlorides and the resulting precipitate
washed with cold water to remove other cations groups.

2. PbCl is removed from the precipitate by leaching with hot water.

3. Separation of AgCl and HgCl with ammonia water.

II. A. Chemical Reagents:


Test Solutions: 3F HCl; 3F HNO; SnCl; NH
3F NHOH ; 1F KCrO; Conc. HNO; HO

II. B. Laboratory Materials:


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

III. Procedures:

A. Precipitation of Group I Cations:

1. Place 10-drops of the test solution in a 10-mL test tube.

2. Add 4 drops of 3F HCl. Mix thoroughly and Centrifuge.

3. To one supernatant liquid, add another drop of 3F HCl to test for complete precipitation.

4. Centrifuge. Then separate the precipitate from the centrifugate. (Save for the
confirmatory test for Pb). C-8.
B. Separation of Group I Cations:

5. To the white precipitate obtained in Procedure A-4, add 6-7 drops of HO and heat for
3-minutes in a water bath.

6. Centrifuge while hot. Remove the centrifugate immediately. The centrifugate will be
analyzed according to Procedure C-9 and the precipitate will be analyzed according to
procedure C-10.

7. Treat the precipitate with 10 drops of NH, stir and centrifuge. Blackening indicates the
presence of Mercurous ion.

C. Confirmatory Test:

C. For Pb

8. To the centrifugate from Procedure A-4, add 4 drops of 1F KCrO.

Positive result:

Yellow precipitate confirms the presence of LEAD.

Chemical Reaction Involved:


Pb + CrO PbCrO

C. For Ag

9. Acidify the centrifugate of Procedure 6, with 3F HNO.

Positive Result:

Formation of white precipitate confirms the presence of SILVER ion.

Chemical Reaction involved:

Ag (NH) + Cl + 2HO AgCl + 2NH + 2HO

C. For Hg

10. To the precipitate (from procedure 7), wash with 10 drops of water. Discard the
Washings.

11. Dissolve the precipitate in 2 drops of conc. HNO.

12. Dilute with5-drops of water. Then add 1-2 drops of SnCl solution.

Positive Result:

White or Gray Precipitate confirms MERCUROUS Ion.

Chemical Reaction Involved:

HgCl + SnCl 2Hg + SnCl


IV. OBSERVATION/S:

V. CONCLUSION/S:

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