Experiment 25

Final-10/5/15

QUALITATIVE ANALYSIS
MATERIALS: 0.1 M solutions of Pb2+, Ag+, Fe3+, Ni2+, and Al3+; a solution that is 0.10 M in all five ions; 6 M
HCl; 3 M NaOH; 1.5 M K2CrO4; 1% Dimethylglyoxime (DMG) in aqueous ethanol; 15 M NH3;
1 M KSCN; unknowns; red and blue litmus paper; test tubes; centrifuge; Bunsen burner.

PURPOSE: The purpose of this experiment is to identify the metal ions present in an unknown solution.

LEARNING OBJECTIVES: By the end of this experiment, the student should be able to demonstrate the
following proficiencies:

1. Conduct chemical tests to determine the presence or absence of specific ions in a solution.
2. Predict the product of a precipitation reaction.
3. Read and follow a flow chart.
4. Construct a flow chart from the results of a given series of chemical reactions.
5. Summarize the results and observations from an experiment into a short laboratory report.

DISCUSSION:

There are two types of problems that are of interest to analytical chemists. One is qualitative analysis, which
is the determination of the presence or absence of a given species in a sample. The other is quantitative analysis,
which is the determination of how much of a species is present in a sample.
This experiment involves the qualitative analysis of solutions containing one or more metal cations. Several
specific reactions will be carried out on solutions that will either separate the ions from each other or confirm the
presence of one particular ion. The reactions that confirm the presence of a particular ion involve the creation of
visible products such as precipitates or colored species. A reaction that results in a precipitation can also be used to
separate ions from the solution.
Qualitative analysis is relatively simple when a solution is known to contain only one ion. For example,
suppose a solution contains either of the ions A2+ or B+. It is known that A2+ reacts with C- to form a yellow
precipitate while B+ combines with C- to form a green precipitate:

A2+ + C- → yellow precipitate

B+ + C- → green precipitate

Identifying which ion is present in solution only requires addition of C- to the solution and observation of the
resultant precipitate color. Difficulty arises if the solution contains both ions. In this case, the combination might
result in a slightly lighter green precipitate, making it difficult to determine if the solution contained only B+ or both
ions. The presence of B+ interferes with the test for A2+ and vice versa.
The strategy for investigating solutions with multiple ions is to first find chemical reactions that will separate
the ions. Once the separation has been accomplished, the ions can be tested and identified individually. For
example, in the case of the A2+ and B+ mixture, it is found that addition of base will result in the formation of
A(OH)2 which is insoluble and precipitates from solution. In contrast, B+ does not react with the base and remains
as an ion in solution.

A2+ + 2 OH- → A(OH)2 (s) precipitate

B+ + OH- → no reaction

Therefore, treating the unknown solution with sodium hydroxide can result in one of the following two situations:

1. No precipitate: The conclusion is that A2+ is not present. Confirm the presence or absence of B+ by
adding C- to the solution and looking for the green precipitate.

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 2. Presence of a precipitate: Separate the precipitate (possibly containing A2+) from the supernatant
(possibly containing B+) by centrifuging the test tube and decanting (pouring off) the supernatant, which
is the liquid above the precipitate. The supernatant is then tested for the presence B+ as described above.
The precipitate should also be tested to verify that it contains A2+ and not some other impurity that
precipitates in base. To do this, dissolve the precipitate in neutral or acidic solution, add C-, and look for
the yellow precipitate.

These possibilities are illustrated in the flow chart shown below.

Unknown solution of
metal ions, A2+ and B+

Add NaOH Separation Process

A(OH)2 Precipitate B+ in Solution

Add HCl Confirming test for

Add C- presence or absence
A2+ in Solution of B+

Green Precipitate
Confirming test for
presence or absence of A2+ Add C-

Yellow Precipitate

Figure 1. Flow Chart for Separation and Identification of A2+ and B+

The lab work for this experiment will be performed over three lab periods. During the first two periods,
conduct the tests described in the procedure with the known solutions provided. Start with the single ion solutions.
Use the observations from these tests to devise a qualitative analysis scheme that will allow for separation of the
ions and identification of the ions present in an unknown. Test the flow chart by using the available solution that
contains all five ions. Carefully record observations for each reaction. While carrying out these reactions, take
specific note of which reactions will separate the ions and which reactions give distinctive products which allow for
the identification of specific ions. For example, there may be only one bright crimson solid produced. Also, note
which ions interfere with the detection of other ions. Making up known mixtures of ions to test may be helpful in
confirming your observations. Once a successful scheme has been developed, determine which specific ions are
present in an unknown solution.
Experiment 25 Time Line

Prior to Lab During Lab Post Lab

Part A – Individual Ions
Week 1 Read the Discussion Develop initial flow chart
Answer In-lab questions
Revise and finalize your
Finish Part A
Week 2 Prepare for lab flow chart; Have your instructor
Part B – Five Ion Solution
check your flow chart

Week 3 Prepare for lab Part C – Unknown Solution Prepare the lab summary

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PROCEDURE:

The chemical reactions (tests) used in this experiment are described below. The reagents are in small
dropper bottles. Be careful not to contaminate any of the reagents.

Carefully record observations for each reaction in the appropriate tables. These observations should
include a detailed description of the appearance of any precipitates (i.e., gelatinous, wispy, deep red,
voluminous, etc.) and any color changes.

Dispose of all solutions in the proper waste containers.

Part A. Qualitative Tests for the Individual Ions

Test I. Chloride Test

1. Clean 5 test tubes. Use a test tube brush to remove any solid material. Rinse the tubes well
with distilled water.
2. Place 10 drops of each individual metal solution (Pb2+, Ag+, Fe3+, Ni2+, Al3+) into its own
test tube. Label the test tubes.
3. Add 5 drops of 6 M HCl to each test tube. Mix the solutions. Record your observations in
the Data Section.
4. a. If a precipitate forms, mix the solution well to allow complete reaction and centrifuge
for 5 minutes. Make sure the centrifuge is balanced before spinning your sample.
Continue with Step 5.
b. If no precipitate forms, dispose of these solutions in the proper waste container.
5. After centrifuging, check the supernatant (the liquid above the precipitate) for complete
precipitation by adding a few more drops of 6 M HCl. If more precipitate forms, centrifuge
again for 2 minutes.
6. Wash the precipitate twice with 10 drops of distilled water. To wash the precipitate,
decant (pour off) the supernatant, add distilled water, and mix well. Centrifuge after
each addition of water and decant. Save the precipitate for use in Test II.

Test II. Hot Water/K2CrO4 Test

A. Hot Water Test
1. Add 15 drops of distilled water to each precipitate from Test I.
2. Heat the test tubes in a boiling water bath for 5 to 10 minutes. While heating, mix the
contents of the test tube often. Did any of the precipitates dissolve? Record your
observations. If the ion did not give a precipitate in Test I, put an X in the corresponding box.
B. K2CrO4 Test
3. a. If a precipitate is still present after heating, centrifuge and save the decanted supernatant.
Add 2 drops of K2CrO4 solution to the hot supernatant.
b. If the precipitate dissolved upon heating, add 2 drops of K2CrO4 to the hot liquid.
4. Record your observations.

Test III. NaOH Test

1. Clean your test tubes. Add 10 drops of each individual metal solution (Pb2+, Ag+, Fe3+,
Ni2+, Al3+) into its own test tube. Label the test tubes.
2. To each test tube, add 1 drop of 3 M NaOH solution, mix well, and note any changes.
Repeat this process until you have added a total of 10 drops of NaOH. Record your
observations.
3. a. If a precipitate remains after the addition of 10 drops of NaOH, mix the contents of the
tube, centrifuge and check the supernatant for complete precipitation. Add 10 more
drops of NaOH if the precipitation was not complete. Wash the precipitate twice with
10 drops of distilled water. To wash the precipitate, decant (pour off) the supernatant, add
distilled water, and mix well. Centrifuge after each addition of water and decant. Save the
precipitate for either Test IV or Test V.
b. If no precipitate forms, dispose of these solutions in the proper waste container.

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Test IV. NH3 Test
1. IN THE HOOD, add 10 drops of 15 M NH3 to the test tubes containing precipitate from
Test III. Make sure to replace the cap on the ammonia reagent bottle after use.
2. Mix 2 minutes and centrifuge. Record your observations. If the ion did not give a precipitate
in Test III, put an X in the corresponding box.

Test V. KSCN Test

1. Repeat Test III for each ion that resulted in a precipitate. Separate and wash the precipitate
well.
2. Add 6 drops of 6 M HCl to the precipitate and mix.
3. Add 2 drops of KSCN solution and mix. Record your observations. If the ion did not give a
precipitate in Test III, put an X in the corresponding box.

Test VI. Dimethylglyoxime (DMG) Test

1. Clean your test tubes. Add 10 drops of each individual metal solution (Pb2+, Ag+, Fe3+,
Ni2+, Al3+) into its own test tube. Label the test tubes.
2. Test the pH of each solution with litmus paper.
3. If the solution is acidic, add 3 M NaOH dropwise until the solution is basic.
4. Once each solution is basic, add 2-4 drops of DMG solution to each test tube and mix.
Record your observations.

Clean Up:
1. Dispose of all waste solutions in the proper waste containers.
2. Clean your test tubes and place them inverted on the test tube rack to drain.
3. Clean all glassware. Return all equipment to their original locations.
4. Check that you have a complete set of reagents and organize the reagents.

Data Analysis
Using your results from Part A and your answers to questions 1-6, devise a qualitative analysis
scheme (flow chart) for analyzing a solution containing all five ions, Pb2+, Ag+, Fe3+, Ni2+, and Al3+.
Questions to think about while constructing your flow chart include:
Does the sequence of the tests matter?
Which test should be done first?
How can I separate the ions?
How can I determine the presence or absence of a particular ion?
Can I unambiguously identify the presence of each of the five ions in the solution? (The
confirming test for the Al3+ ion may be a bit challenging.)

Draw your initial flow chart on the appropriate page of the Data Analysis Section. Prior to commencing
further work in the laboratory, discuss your flow chart with your instructor.

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Part B. Qualitative Analysis Scheme and Qualitative Tests for Five Ion Solution

After your scheme has been approved, test it by analyzing the “Five Known Ion” solution. Based upon
your experimental results, make revisions to your scheme, if necessary. Include your improved flow chart
on the appropriate page of the Data Analysis Section and show your final version to your instructor.

Part C. Analysis of an Unknown Solution

Once your instructor has approved your final flow chart, obtain an unknown solution and record its
number in the Data Section. Use your flow chart to help you analyze your unknown solution. Determine
which ions are present in your unknown by conducting chemical tests and providing experimental support
for your determination. Record your lab procedure including your experimental results and observations on
the appropriate page in the Data Analysis Section.

Written Lab Summary:

After completing this experiment, summarize your results in a short abstract or executive summary.
This type-written summary must be a concise, organized, and readable description of your lab results which
address the following areas:

1. Purpose
What problem are you trying to solve in this experiment?
2. Experimental Methods
Provide a brief overview of the lab protocols you used. Summarize your flow chart.
3. Results
Briefly summarize your experimental results.
How did you solve your problem?
What ions were present in your unknown?
Explain how you reached your conclusions.
Your experimental results should support your claims.
4. Discussion/Conclusion
What sources of error exist in this experiment?
Why is qualitative analysis important?

Limit your summary to one or two type-written pages. Additional information on writing abstracts can be
found at https://owl.english.purdue.edu/owl/resource/656/01/ .

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