Zackary Park

Wei Chen
Experiment 12: Qualitative Analysis of Cations
Th 530-830
February 13, 2014
Questions
1. Write out the procedure that you followed in lab to separate the four cations. Write it in a
step by step manner so that someone else performing the experiment could follow it.
1. Place in a test tube about 15 drops of a solution containing, containing some, or not containing
the four cations: ZrO2+ (aq), Ni2+ (aq), Pb2+ (aq), and Al3+ (aq).
2. Add 12 drops of 6 M HCl (aq) to the test tube. HCl (aq) will react with Pb2+ (aq) to form a
precipitate. The other cations, ZrO2+ (aq), Ni2+ (aq), and Al3+ (aq), are soluble in HCl (aq), meaning
that they will not form a precipitate.
3. Stir the solution thoroughly for 2 minutes using a stirring rod. Place the test tube in an ice bath
for 5 minutes. After complete precipitation, centrifuge the test tube for 5 minutes to separate the
precipitate and the aqueous cations. Test the solution with litmus paper. It should be very acidic.
Decant the supernatant solution into another test tube, which will be used later. If no precipitate has
formed, then Pb2+ (aq) is not present in the original solution.
4. Wash the precipitate using deionized water. Decant the rinse water, and dispose of it
accordingly. Repeat this process. To confirm the presence of lead, add 10 drops of water to the test
tube containing the precipitate. Fill a beaker with water, and place it on a beaker with the heat on
high. Place an aluminum test tube cover over the beaker, and put the test tube through the hole.
Wait 5 minutes for the water to boil. Be sure the heat caused the precipitate to dissolve completely.
5. Add 2 drops of acetic acid and 4 drops of 0.1 M potassium chromate. The formation of a bright
yellow precipitate confirms the presence of Pb2+ in the original solution.
6. The supernatant solution set aside contains the cations, ZrO2+ (aq), Ni2+ (aq), and Al3+ (aq). Add
12 drops of 6 M NaOH (aq) to the test tube. NaOH (aq) will react with Ni2+ (aq) and ZrO2+ (aq) to
form a precipitate. The other cation, Al3+ (aq), is soluble in NaOH (aq).
7. Stir the solution thoroughly for 2 minutes using a stirring rod. Place the test tube in an ice bath
for 5 minutes. After complete precipitation, centrifuge the test tube for 5 minutes to separate the
precipitate and the aqueous cation. Test the solution with litmus paper. It should be very basic.
Decant the supernatant solution into another test tube, which will be used later. If no precipitate has
formed, then Ni2+ (aq) and ZrO2+ (aq) are not present in the original solution.
8. Wash the precipitate using deionized water. Decant the rinse water, and dispose of it
accordingly. Repeat this process. To confirm the presence of nickel or zirconyl, add 12 drops of 6
M HCl (aq) to the test tube containing the precipitate. Stir the solution thoroughly for 2 minutes
using a stirring rod. The precipitates will dissolve, forming the cations, ZrO2+ (aq) and Ni2+ (aq)
into the solution.
9. Add 12 drops of 6 M NH3 (aq) to the test tube. NH3 (aq) will react with ZrO2+ (aq) to form a
precipitate. The other cation, Ni2+ (Aq), is soluble in NH3 (aq).
10. Stir the solution thoroughly for 2 minutes using a stirring rod. Place the test tube in an ice bath
for 5 minutes. After complete precipitation, centrifuge the test tube for 5 minutes to separate the
precipitate and the aqueous cation. Test the solution with litmus paper. It should be very basic.
Decant the supernatant solution into another test tube, which will be used later.
11. Wash the precipitate using deionized water. Decant the rinse water, and dispose of it
accordingly. Repeat this process. To confirm the presence of zirconyl, add enough drops (~20
drops) of 6 M HCl to the test tube to make the solution acidic. Test it with litmus paper. Add 2
drops of Alizarin Red solution. Test the solution again to confirm it is still acidic.

Zackary Park
Wei Chen
Experiment 12: Qualitative Analysis of Cations
Th 530-830
February 13, 2014
12. Fill a beaker with water, and place it on a beaker with the heat on high. Place an aluminum test
tube cover over the beaker, and put the test tube through the hole. Wait 2 minutes. The formation
of a red-violet color indicates the presence of ZrO2+ (aq) in the original solution.
13. One of the supernatant solutions set aside contains Ni2+ (aq). Add 12 drops of 6 M NaOH (aq)
to the test tube. NaOH (aq) will react with Ni2+ (aq) to form a precipitate. 14. Stir the solution
thoroughly for 2 minutes using a stirring rod. Place the test tube in an ice bath for 5 minutes. After
complete precipitation, centrifuge the test tube for 5 minutes to separate the precipitate and the
aqueous cation. Test the solution with litmus paper. It should be very basic. Decant the
supernatant, and dispose of it accordingly.
15. Wash the precipitate using deionized water. Decant the rinse water, and dispose of it
accordingly. Repeat this process. To confirm the presence of nickel, add enough drops of 6 M HCl
(aq) to dissolve the precipitate. Then add enough drops of 6 M NH3 (aq) to make the solution very
basic. Confirm this by testing the solution with litmus paper. Add 1 drop of 1% DMG solution.
The formation of a cherry-red precipitate indicates the presence of Ni2+ (aq) in the original solution.
16. In the first supernatant solution that was set aside, it contains Al3+ (aq). Add12 drops of 6 M
NH3 (aq). NH3 (aq) will react with Al3+ (aq) to form a precipitate.
17. Stir the solution thoroughly for 2 minutes using a stirring rod. Place the test tube in an ice bath
for 5 minutes. After complete precipitation, centrifuge the test tube for 5 minutes to separate the
precipitate and the aqueous cation. Test the solution with litmus paper. It should be very basic.
Decant the supernatant, and dispose of it accordingly.
18. Wash the precipitate using deionized water. Decant the rinse water, and dispose of it
accordingly. Repeat this process. To confirm the presence of aluminum, add enough drops of 6 M
HCl to dissolve the precipitate and to make the solution very acidic. Confirm this by testing the
solution with litmus paper.
19. Add 2 drops of 0.1% aluminum solution and enough drops of 6 M NH3 (aq) until the solution
becomes basic. Confirm this by testing the solution with litmus paper. Stir the solution thoroughly
for 2 minutes using a stirring rod. If a red-pink precipitate forms, Place the test tube in an ice bath
for 5 minutes. After complete precipitation, centrifuge the test tube for 5 minutes to separate the
precipitate and the aqueous cation. Decant the supernatant, and dispose of it accordingly.
20. Add 3 drops of 6 M NaOH to the solid. The precipitate will dissolve, and the formation of a
clear magenta solution indicates the presence of Al3+ (aq) in the original solution.
2. Write balanced molecular equations for the formation of any precipitates that appeared
upon addition of HCl or NaOH when testing the solubilities of the cations (refer to your
solubility table). [Use NO3 as the anion in the formulas for the metallic compounds.]
2 HCl (aq) + Pb(NO3)2 (aq) 2 HNO3 (aq) + PbCl2 (s)
2 NaOH (aq) + ZrO(NO3)2 (aq) 2 NaNO3 (aq) + ZrO(OH)2 (s)
2 NaOH (aq) + Ni(NO3)2 (aq) 2 Na(NO3) (aq) + Ni(OH)2 (s)
3. What is the chemical formula for the yellow precipitate that is obtained in the
lead confirmation test? Write a balance molecular equation for this reaction,
using NO3 as the anion in the lead compound. Note: Do not include acetic 3
acid in the equation. It is present because the precipitate is very insoluble in acetic acid.
Pb(NO3)2 (aq) + K2CrO4 (aq) 2 KNO3 (aq) + PbCrO4 (s)