Qualitative Analysis – Determination of Cations and Anions

I. Objectives
1. To record observable results for elimination and confirmatory tests for all cations
and anions in solutions from the experiment video.
2. To deduce presence or absence of ions in aqueous solutions using the results
recorded.
3. To balance chemical equations and net ionic equations representing reactions in the
qualitative tests.
4. To identify ions in an unknown solution using the results from the qualitative
analysis.

II. Outline/Schematic diagram of procedure:

1. Qualitative analysis of known ions

TEST FOR CATIONS

Prepare 5 clean and dry test tubes for qualitative test for cations.

Place 5 drops of Cu2+, Fe3+, Ca2+, Zn2+, and NH4+ solutions

separately into separate 5 test tubes.

Add a drop of 1.0 M NaOH into each of test tubes.

If a precipitate form, continue adding NaOH dropwise until

precipitation is complete (does not produce precipitates).

Note the color and type of precipitate formed.

Adding excess NaOH to the precipitates (about 5-10 drops more).

A-1. Elimination tests for cations using NaOH

Prepare 5 clean and dry test tubes for qualitative test for cations.

Place 5 drops of Cu2+, Fe3+, Ca2+, Zn2+, and NH4+ solutions

separately into separate 5 test tubes.

Add a drop of 1.0 M NH3 into each of test tubes.

If a precipitate form, continue adding NH3 dropwise until

precipitation is complete (does not produce precipitates).

Note the color and type of precipitate formed.

Adding excess NH3 to the precipitates (about 5-10 drops more).

A-2. Elimination tests for cations using NH3

B-1. Confirmatory tests for copper (II) ion, Cu2+

Mix Cu2+ solution in A-2 with excess NH3.

If deep blue complex is obtained, note with presence of Cu2+.

Add 2 drops of 0.1 M KSCN to 5 drops of the fresh Fe3+ solution.

If red blood complex is obtained, note with presence of FeSCN2+.

Add 2 drops 0.1 M K4Fe(CN)6 to 5 drops of the fresh Fe3+ solution.

If with dark blue precipitate, note with presence of KFeIIIFeII(CN)6.

B-2. Confirmatory tests for iron (III) ion, Fe3+

B-3. Confirmatory tests for calcium (II) ion, Ca2+

Add drops of 0.1 M (NH4)2C2O4To 5 drops of Ca2+ test solution.

A white precipitate will be obtained

B-4. Confirmatory tests for zinc (II) ion, Zn2+

Add 2 drops of 0.1 M K3Fe(CN)6 to 5 drops of the Zn2+ test tube.

A yellow precipitate, KZnFe(CN)6, will be obtained.

Add 2 drops 0.1 M K4Fe(CN)6 to 5 drops of the Zn2+ test tube.

A white precipitate, K2Zn3[Fe(CN)6]2, will be obtained.

Moisten 2 small pieces of litmus paper (red and blue) with distilled
water and allow to stick to underside of watch glass.

Place 10 drops of NH4+ test solution in evaporating dish.

Add 5 drops of NaOH to the test solution.

Cover evaporating dish with the evaporating dish immediately.

Observe as the red litmus paper turns blue.

B-4. Confirmatory tests for ammonium ion, NH4+

TEST FOR ANIONS

C-1. Elimination tests for anions using Ba(NO3)2
Prepare 7 clean and dry test tubes for qualitative test for cations.

Prepare clean and dry test tubes for qualitative test for cations.
Place 5 drops of CO32-, SO42-, PO43-, I-, SCN-, Br-, and NO3- solutions
separately into separate 7 test tubes.
Place 5 drops of anion solutions separately into separate test tubes.

Add 2 drops of 1.0 M Ba(NO3)2 into each of test tubes.

Add 2 drops of 1.0 M HNO3 into each of test tubes.

If precipitate form, add Ba(NO3)2 until precipitation is complete

Add 3 drops of 0.1 M Fe(NO3)3 and 5 drops of toluene.

Decant supernatant after precipitates settle.

Shake and allow immiscible layers to stratify.

Set precipitates aside for Part D.

Add few drops of toluene if color is difficult to see.

Record color of each layer.

C-2. Elimination tests for anions that did not form precipitates with Ba(NO3)2
C-3. Elimination tests for anions that did not form precipitates with Ba(NO3)2
Prepare clean and dry test tubes for qualitative test for cations.

Place 5 drops of anion solutions separately into separate test tubes.

Add 2 drops of 1.0 M HNO3 to KMnO4 solutions to acidify.

Add 1 drop of 0.01 M acidified KMnO4 and 5 drops of toluene.

Shake and allow mixture to stratify.

Record color of each layer.

D-1. Confirmatory tests for carbonate ion, CO32-

Add 1.0 M CH3COOH until precipitate from C-1 is immersed.

If precipitate dissolves with effervescence, note with

presence of CO32- as conversion to gas.

Add 1.0 M CH3COOH until precipitate from C-1 is immersed.

If precipitate dissolves without effervescence, note with

presence of PO43-.

Add 1 drop of 1.0 M MgCl2 to PO43- test solution.

If white precipitate forms, note with presence of PO43-.

D-2. Confirmatory tests for phosphate ion, PO43-

D-3. Confirmatory tests for sulfate ion, SO42-

Add 5 drops of 1.0 M CH3COOH to precipitate from C-1.

If precipitate remains undissolved after addition of acetic

acid, note with presence of SO42-.

D-4. Confirmatory tests for iodide ion, I-

If a pink or pinkish-red color of the toluene layer is observed
in C-2, note with presence of I-.

D-5. Confirmatory tests for thiocyanate ion, SCN-

If deep red aqueous solution is observed in C-2, note with
presence of SCN- as it is FeSCN2+

D-6. Confirmatory tests for bromide ion, Br-

If yellow or orange toluene layer C-3 is observed, note with
presence of Br-.
 D-7. Confirmatory tests for nitrate ion, NO3-

Acidify solution by adding 6 drops of 6.0 M H2SO4.

Add 8 drops of freshly prepared FeSO4.

Add 2 drops of 18.0 M H2SO4 by tilting the test tube.

Do not shake test tube. Bring test tube in upright position carefully.

If formation of brown ring at the interface of acid is observed,

note with presence of NO3-.

Record information regarding unknown solution.

Dilute the solution with distilled water at own discretion.

Use solutions for every qualitative test. Identify ion.

2. Analysis of unknown ions in solution

III. Special Notes (proper waste disposal, safety precautions):

A. Waste disposal
1. Dispose all solutions of inorganic salts by diluting them with plenty of water and
flushing them directly down the sink with copious running water.
2. Dilute acidified and basic solutions with water when needed, before flushing them
down the sink.
3. Dispose excess concentrated acids into the acid waste container.
4. Dispose solutions containing KMnO4 into the inorganic waste container, or to the
KMnO4 waste container.
5. Dispose all undissolved solids into the solid waste container. Place and wrap these
precipitates in a filter paper or tissue before throwing them into the solid waste jar.
 6. Pour all mixtures with layering into a separatory funnel. Separate the toluene layer
from the aqueous layer.
7. Dispose the toluene layer into the halogenated organic waste jar. Dispose the
aqueous layer into the inorganic waste jar.

B. Safety Precautions
1. Use of Personal Protection Equipment (safety glasses, gloves, protective clothing,
face shield, masks, laboratory gowns and closed shoes)