PROCEDURE (Act.

1)

1. On your worksheet copy the names and formulas of the compounds to be tested.

2. Obtain a wire loop and spot plate. Label your spot plate with each of the test solutions.

Label the unknown as well. Obtain the unknown number you will be working on from your

instructor.

3. Obtain 10 - 15 mL of 6 M HCl in a 50 mL beaker. This will be used to rinse your loop.

4. Add 3 drops of each of the known solutions or a pinch of crystal of the unknown solid to

separate wells in your spot plate. Be sure to match the solution to the properly labeled

well!

5. Set up and prepare your alcohol lamp.

6. Clean the wire loop as follows: Dip the loop end of the wire loop into the HCl(aq) in the

beaker and stir the acid gently for a few seconds. Then heat it in the hottest part of the

alcohol lamp flame until it glows. If a burst of color is observed, repeat the HCl cleaning.

When no color is imparted to the flame, the wire is clean. You may have to repeat this

process a couple of times. Note that the acid wash accomplishes the cleaning, so give

extra attention to this procedure. Also, some clean wires impart a pale-yellow color to the

flame.

7. Dip the clean metal loop into the well of the solution to be tested and bring the loop

(slowly) to the hottest portion of the flame. Observe and record in Table A the color

observed in the flame. Watch carefully since some colors are very fleeting while others

last a relatively long time. Color descriptions might include the bright red, deep red,

orange-red, orange, yellow, yellow-green, green, blue, and violet.

8. Repeat steps 4 and 5 for each of the known solutions; from the data, determine which of

the ions present are responsible for the color noted.

9. Test the unknown solutions in the same manner and identify the ions in the unknown.

You may wish to look at one or more of the known solutions again if you are not

completely sure of the identity of the unknown.

Perform each test for each of the anions stock solutions as directed. Repeat each test using a

solution made by diluting the anion solution 9:1 with distilled water. Ensure to mix well before

performing the analysis. A boiling-water bath containing about 100 mL of water in a 150-mL

beaker will be needed in some tests. Make sure to set this up before proceeding.

A. Test for the Presence of Carbonate Ion, CO32-

Carefully add 1 mL of 6M HCl to 1 mL 1M Na2CO3 in a small test tube. Observe the formation

of bubbles which indicates the evolution of carbon dioxide gas. Effervescence is much less

obvious for a dilute solution, and warming in a water bath, with stirring, will increase the amount

of bubble formation.

B. Test for the Presence of Sulfate Ion, SO42-

Add 1 mL of 6M HCl to 1 mL of 0.5 M Na2SO4. Add a few drops of 1 M BaCl2. Note down your

observations.

C. Test for the Presence of Phosphate Ion, PO43-

Add 1 mL 6 M HNO3 to 1 mL 0.5 M Na2HPO4. Then add 1 mL of 0.5 (NH4)MoO4 and stir

thoroughly. A yellow precipitate will form to indicate the presence of the phosphate ion. The

solid may form slowly, especially in dilute solution. Putting the test tube in a boiling water bath

for a few minutes can aid in precipitate formation.

D. Test for Presence of Sulfite Ion, SO32

Add 6M HCl to 1 mL of 0.5M Na2SO3. Carefully, using proper procedure, sniff the rod to

try to detect the acid odor of SO2. If the odor is too faint to detect, put the test tube n a hot water

bath for 10 seconds and sniff again.

E. Test for the Presence of Thiocyanate Ion, SCN-

Add 1 mL of 6M acetic acid, HC2H3O2, to 0.5 M KSCN and stir. Add one or two drops of
0.1M Fe(NO3)3. A deep red coloration should be observed due to the formation of FeSCN2+ ion if

SCNion is present.

F. Test for the Presence of Chloride Ion, Cl-

Add 1 mL of 6M HNO3 to 1 mL of 0.5M NaCl. Add two to three drops of 0.1 M AgNO3. A

milky white precipitate should form.

Note: SCN- will interfere with this reaction. Remove SCN- by adding 1 mL of HNO3 to 1 mL of the

solution and then boil gently until the volume is reduced to half. This will destroy the thiocyanate.

Cool the solution and proceed with the test.

G. Test for the Presence of Acetate Ion, C2H3O2-

1. Slowly, drop by drop, add 6M NH3 or 6M HNO3 to 1 ml of 0.5M NaC2H3O2 until the

solution is just basic with litmus test.

2. Then, add 1 drop of BaCl2 to eliminate interfering ions. If a precipitate forms, add 1 mL

of the BaCl2 to completely precipitate the interfering ions. Centrifuge the mixture.

3. Add another drop of BaCl2 to the undisturbed centrifuged mixture to ensure that no

more precipitation occurs. Repeat step 2 if precipitation still occurs.

4. After completely precipitating out the interfering ions, pipette out 1 mL of the

supernatant liquid into a new test tube, then add to it dropwise 1 mL of 0.1M KI, or until the

solution develops a fairly strong rust color.

5. Add 0.5 mL of 0.1M La(NO3)3 and six drops of 6M NH3. Stir and put the tube in a water

bath. The mixture should darken to a nearly black color after a few minutes.

H. Test for the Presence of Nitrate Ion, NO3-

1. Add 1 mL 6M NaOH to 1 mL of 0.5M NaNO3. Then add a few granules of Al metal using

a spatula. Put this in a hot water bath.

2. Observe the solution for a few seconds. The Al-NaOH reaction will produce H2 gas,

which will reduce the NO3-

paper just above the end of the test tube. This should gradually turn blue within a minute or two.

3. Cautiously sniff the vapors at the top of the tube. The odor of ammonia should be

detectable.

Note: the SCNion will interfere with this test. To eliminate the presence of SCN-, add 1 mL CuSO4

to 1 mL of the sample and place it in a hot water bath for 2 minutes. Centrifuge. Pipette out 1 mL

of the liquid without disturbing the precipitate. Add 1 mL of 1M Na3CO3 to the liquid to remove

excess Cu2+ ions. Centrifuge. Pipette out 1 mL of the liquid into a test tube and begin with the test

from step 1.

I. Unknown Solution

When you have completed the tests, obtain your unknown number from your instructor.

Each unknown solution contains two (2) anions. Identify the anions in your unknown using the

tests you just performed above.

PROCEDURE

Step 1. Separation of Group 1 cations from a mixture

Qualitative analysis of metal cations begins with separation by precipitation of the group

1 cations. In this experiment, the positive control is a solution of equal volumes of 0.1M AgNO3,

0.2M Pb(NO3)2, and 0.1M Hg2(NO3)2.

Add 2 drops of 6M HCl to 1 mL of the sample solution. Mix with a stirring rod. Centrifuge

the mixture. (The proper use of centrifuge will be demonstrated. Do not proceed unless you have

learned the equipment operation.) Check for completeness of precipitation by adding one more

drop of 6M HCl to the centrifuged mixture. Decant the supernatant, which should contain other

cations groups if present, into another test tube and save.

Wash the precipitate from Step 1 by adding 1 to 2 mL water, stir, centrifuge and decan

the supernatant. This liquid can be discarded. Add 2 mL of distilled water to the washed

precipitate and place the tube in a boiling water bath. Leave this for 1-2 minutes with occasional

stirring. Centrifuge the hot mixture and decant the supernatant to a new test tube. This will

contain the dissolved Pb2+ ions. Save the residue for further testing.

Step 3. Confirmatory test for Pb2+

To the liquid in Step 2, add 1 drop of 6M Acetic acid (HC2H3O2) and a 3-5 drops of 0.1M

K2CrO4. A bright yellow precipitate of PbCrO4 will form to confirm the presence of Pb2+.

Step 4. Separation and Confirmatory test for Hg2 2+

Add 1 mL of 6M NH3 to the precipitate in Step 2 and stir thoroughly. A gray to black

precipitate forms from the reaction of Hg2 2+ with NH3 will form. Centrifuge the mixture and decant the
liquid into a new test tube.

Step 5. Confirmatory test for Ag+

Add dropwise 6M HNO3 to the solution in Step 4 until the solution is acidic by litmus test.

If the solution is sufficiently acidic, Ag+ will form a white precipitate for AgCl. AgCl is insoluble in

an acidic medium and this is a characteristic property of the solid used for its separation.

Step 6. Unknown analysis

Apply the analysis flow for your positive control to the unknown solution provided by your

instructor.