ANALYSIS OF GROUP IV CATIONS

1. Prepare known solution by mixing approximately 1 ml each of magnesium nitrate, barium nitrate,

strontium nitrate and calcium nitrate.

2. Dilute with distilled water to approximately 10 ml (6ml of Distilled Water).

Analyze as a practice unknown by the following procedure:

Precipitation of Group IV( Ba2+,Sr2+,Ca2+,Mg2+)
1. To 3 ml of the unknown solution in a vial add 1 ml of 5 M NH4Cl

2. Then add 15 M  NH4OH drop by drop until basic and add 3 drops in excess.

3. Heat the solution almost to boiling but do not boil.

4. Add 1 ml of (NH4)2CO3 reagent

5. Mix and allow the solution to stand for at least five minutes

6. Centrifuge.

7. Test for completeness of precipitation by adding a few drops of the ammonium carbonate reagent.

(If a cloudiness forms around the drops of reagent added, stir the solution, warm gently, and then-centrifuge
again.)
8. Test again for completeness of precipitation.

9. When precipitation is complete decant the supernatant liquid which may contain magnesium ion and

group V ions and treat it by procedure C.

(Use this supernatant liquid to test for potassium by A-4). (Wash the precipitate with two 2 ml portions of water
and discard the washings.)

ppt: BaCO3, SrCO3, CaCO3 Sol’n: Mg2+

Test for Barium Ion: (ppt: BaCO3, SrCO3, CaCO3)

1. To the precipitate add 6 MHAc dropwise until the solid is just dissolved, or until 10 drops of the HAc

solution have been added.

 2. Then add a number of drops of 3 M NH4Ac equal to the number of drops of HAc used in dissolving the

precipitate.

3. Dilute the solution to 2 ml with water.

4. Heat the solution to boiling and add one drop of 1 M K2CrO4

5. Discard the solid and save the supernatant liquid.

6. Centrifuge.

(If no precipitate forms barium is absent and the solution is treated by B-2.)
(If a precipitate forms, heat again and add a second drop of 1 M K2CrO4. Centrifuge.)

7. Before decanting the supernatant liquid observe to see that it is yellow.

(If the solution is colorless, heat to boiling, add a third drop of 1 M K2CrO4. Centrifuge.)

8. When the supernatant liquid is yellow decant it and heat it by B-2.

9. Wash the precipitate with two 1 ml portions of water and discard the washings.

ppt: BaCrO4 Sol’n: Sr2+, Ca2+

10. To confirm the presence of barium, dissolve the yellow precipitate in 1 ml of 6M HCI.

Ba2+
11. Apply the flame test.

12. To the remaining solution add two drops of 6 M H2SO.

13. A white precipitate confirms barium Ion.

(If the color of the solution makes the precipitate appear yellow, centrifuge and discard the supernatant liquid.)

14. Wash the precipitate with 1 ml of water.

15. Centrifuge again to as certain whether the precipitate is white.

BaSO4

Test for Strontium Ion:( Sol’n: Sr2+, Ca2+)

 1. Adjust the volume of solution B-2 to about 2ml by either evaporation or dilution.

2. Add 15 drops of triethanolamine

3. Stir with a rod until the solution is homogeneous.

4. Add 1ml of 2M (NH4)2SO4, stir again, and heat to boiling.

5. Centrifuge and examine the bottom of the tube.

6. A white precipitate indicates the presence of strontium ion.

ppt: SrSO4 Sol’n: Ca2+ (Complex)

7. Decant the supernatant liquid through a filter and save the filtrate for B-3.

8. To confirm strontium, wash the precipitate with two 1ml portions of water.

9. Discard the washings.

10. To the washed precipitate add 1ml of ammonium carbonate reagent.

11. Heat and stir.

12. Centrifuge and discard the centrifugate.

ppt: SrCO3
13. Wash the precipitate with two 1ml portions of water and discard the washings:

14. Dissolve the residue in three drops of 6M HCI and make a flame test on the solution.

15. A deep red flame confirms strontium.

Sr2+ - Flame Test (Deep Red Or Crimson Red Flame)

Test for Calcium Ions: (Sol’n: Ca2+ (Complex))

1. To the filtered solution B-3 add 10 drops of 0.2 M (NH4)2C2O4.

2. Centrifuge, decant and discard supernatant liquid.

3. Heat the precipitate with the full heat of the burner then allow the tube to cool.

ppt: CaC2O4
4. Add three drops of 6 M HCI to the residue and carry out the flame test.

Ca2+ -Flame Test (Brick Red Or Orange Red Flame)

(An orange red flame confirms calcium ion.)

(For those who find the color of the calcium flame difficult to distinguish, the white precipitate with ammonium

oxalate may be the more reliable test.)

Test for Magnesium Ions:(Sol’n: Mg2+)

1. To the centrifuge C add five drops of 15 M NH4OH.

2. Add 20 drops of 0.5 M Na2HPO4 solution.

3. Mix and allow to stand for at least 10 min.

4. Centrifuge and discard supernatant liquid.

5. Wash the ppt. with two 1 ml portions of water and discard the washings.

ppt: MgNH4PO4
 6. Dissolve the ppt, in three drops of 6M HCI and dilute with 2 ml water.

7. Add one drop of S and O reagent

8. Warm the solution slightly.

9. Add 6 M NaOH dropwise until the dye turns purple.

(A bright blue ppt. is a positive test for magnesium.)

10. If the color of the solution obscures the color of the ppt.

11. Centrifuge and discard the supernatant liquid.

12. Suspend the ppt. in 1 ml of water containing three drops of 6 M NaOH and note its color.

(Note: If the S and O reagent is not available the formation of a white ppt. with NaOH will confirm

magnesium.) ‘

Mg(OH)2 (White) + Dye (Blue)