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SEPARATION AND IDENTIFICATION

OF GROUP II CATIONS

Sandra C. Ganzo
Christian Marie Araceli P. Solis
INTRODUCTION

 Group II Cations
 Ions that form acid-insoluble sulfides
 Includes Cd2+, Bi3+, Cu2+, As3+, As5+, Sb3+, Sb5+, Sn2+,
Sn4+, Hg2+, andPb2+
 Reagents often used are those that give (S2−) ions
in solution [ex: thioacetamide (CH3 CSNH2 ) and
H2S ]
METHODOLOGY
STEP ONE: Precipitation of Cations as Sulfide
Check pH of centrifugate from A-1: SHOULD BE
0.1. If not, + 6M NaOH/HCl dropwise.

+ 2 mL 5% thioacetamide. Stir.

Heat in boiling water bath for 10 minutes.

If no ppt, PROCEED TO PART C.


If with ppt, and BLACK, Group II cations are PRESENT!
METHODOLOGY

Too acidic – incomplete precipitation


Too basic – precipitation of Group III cations
METHODOLOGY
Cool mixture, decant, and centrifuge.

+ 2 mL 1 M NH4Cl and 2 mL H2O to ppt and set


aside.

Check decanted solution if it is still 0.5. (+ 0.5 NaOAC


if too low, + 0.5 M HOAc if too high).

Heat for 3 minutes, cool, centrifuge, and decant.

Save decantate for part C.


METHODOLOGY
+ 1 mL 1M NH4Cl and 1 mL H2O to precipitate.
Stir.  first part of Group II precipitate.

Stir, centrifuge, decant, discard liquid. Reserve ppt


for step 2.
METHODOLOGY
STEP TWO: Separation of Mixed Sulfide Ppts
+ 15 drops 6 M HNO3  residue from step 1. Heat in
water bath.

Separate and discard sulfur formed.

+ 2-3 drops 6 M HCl clear solution


WHITE PPT: may contain LEAD.

Centrifuge & decant mixture. Reserve residue (for


step 3) and decantate (for step 4).
METHODOLOGY
STEP THREE: Lead Test
To residue from step 2, add 10 drops NaAc.

Heat gently, if necessary to dissolve ppt.

clear solution +1M K2CrO4

POSITIVE FOR LEAD (Pb2+) :


YELLOW PPT
METHODOLOGY
STEP FOUR: Copper Ion Test
To decantate from step two, add 6M NH3 until
basic.
DEEP BLUE SOLUTION: may contain Cu2+.

Divide solution into two.

To ½ , add 6M CH3COOH until color change and it


becomes acidic.

+ 1 drop 0.2 M K4Fe(CN)6


METHODOLOGY
STEP FOUR: Copper Ion Test

POSITIVE FOR COPPER (Cu2+) :


RED PPT
METHODOLOGY
STEP FIVE: Cadmium Test
To the other half of decantate on step 4, if blue,
add pinch of solid Na2S2O4 (sodium
hydrosulfite).

Put test tube into boiling water bath.

Centrifuge residue and discard.


METHODOLOGY
STEP 6: Cadmium Test

Add 2 mL 5% thioacetamide to liquid/ original


colorless decantate in step four.

Heat in water bath.

POSITIVE FOR CADMIUM (Cd2+)


YELLOW PPT
RESULTS: Cations as Sulfides
ION COLOR OF PRECIPITATED COLOR OF THE
SOLUTION OF ION FORM OF ION PRECIPITATE

Hg2+ Colorless HgS Black


Pb2+ Colorless PbS Black
Bi3+ Colorless Bi2S3 Brown to Black
Cu2+ Blue CuS Black
Cd2+ Colorless CdS Yellow
As3+ Colorless As2S3 Yellow
Sb3+ Colorless Sb2S3 Orange
Sn4+ Colorless SnS2 Yellow
EXPECTED RESULTS

POSITIVE FOR LEAD (Pb2+) :


YELLOW PPT

POSITIVE FOR COPPER (Cu2+) :


RED PPT
POSITIVE FOR CADMIUM (Cd2+)
YELLOW PPT
NOTES
 The test with sulfide ion must be conducted with
dilute HCl to keep sulfide ion concentration at a
minimum so as to allow precipitation of group
II cations only. Failure to do this might lead to
the early precipitation of 4th group cations that
might be present  inaccurate results  A NO-
NO!
REFERENCES

 http://www.scribd.com/doc/30014011/Group-
2-and-5-Cation-Analysis
 http://www.docstoc.com/docs/30019542/GR
OUP-II-CATIONS---Photo-gallary

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