Analysis of cations

A Qualitative Analysis of a Mixture of Cations

This experiment involves a type of chemistry called analytical chemistry. Analytical
chemistry deals with analyzing matter. There are two types of this analysis: qualitative and
quantitative. The former deals with what a substance contains. The latter deals with how much
of each constituent is present.
In this lab, we will be doing a qualitative analysis of cations that are dissolved in solution.
In order to do this, we will first separate and then detect the different ions in solution. To
separate and detect these ions, we will perform different chemical reactions on the ions. You are
not expected to fully understand the reactions yet, but you need to be able to identify the different
ions that are reacting, and to predict what may be happening.
The lab contains two parts. The first is to do an analysis of a known solution of cations.
This will offer the chemist a practice run to see what the reactions look like, and how to do an
analysis of aqueous cations. The second part of the lab will be to determine what metals are in
different samples of metal alloys by dissolving the metal and then performing a qualitative
analysis on the solution.
Purpose
The purposes of the lab are:

to separate and confirm the identity of various cations in solution;

to practice formula writing, naming chemicals, and writing chemical equations;

to make careful observations;

to identify what metals constitute an alloy.
Hypothesis
For the hypothesis, define the following words:
 Qualitative analysis, precipitate, solute, solvent, solution, decant, supernatent liquid,
confirming test, centrifuge, pH, reagent, alloy.
Materials You do not need a materials list for this lab.
General information
You will need to be able to identify precipitates and precipitation reactions for this lab.
Use the solubility rules to help to understand the chemistry of what is happening with each step.
It is possible to write a chemical reaction for most of the steps, especially if a solid is created.
Sometimes a precipitate sinks right to the bottom. Other times the particles are small,
and remain suspended, making the solution look cloudy. In order to separate the solid precipitate
out, centrifuge the mixture.
1. Cleanliness is imperative. If glassware is not clean, contamination can occur. Impurities can
cause false confirming tests or unwanted reactions.
2. Washing the precipitate is a technique to make sure that impurities are removed from the
collected solid. Do this by adding a few drops of deionized water, mixing, centrifuging, and then
decanting the wash water.
3. PH testing tests the concentration of the hydronium ion, H+. When testing the pH with pH
paper, dip a stirring rod or pipette into the solution and then touch the rod or pipette to the pH
paper. Do not dip the pH paper into your test tube! PH paper can be used over and over.

Analysis of cations

4. Safety. Keep your goggles on. Protect your eyes (with goggles) and clothes (with aprons).
Clean up spills, and wash your hands if you get anything on them. Many of the chemicals we are
using are very strong acids or bases, and can cause severe tissue damage. Safety violations will
not be tolerated.




Dont directly smell vapors or gases. Waft!

Be careful when heating liquids. Gentle heat is good, a rolling, bumping boil is not.
When in doubt, ask!

Experimental Section
We will be separating out each cation as a solid, testing the solid, and then separating out another
cation as a solid from the liquid that is left over (supernatent liquid). It is important to never toss
anything unless you are sure you do not need it! Be sure to follow the directions carefully, and
label test tubes very, very well. Please read this paragraph twice.
The cations can be separated out using three major steps. The solution is combined with a
reagent that produces a precipitation reaction with a specific cation. The three major steps are
listed below.

Group # (or step #)

Reagent used

Cation precipitated

I
II

HCl(aq)
NH4OH(aq) (aka
NH3 or ammonia)
KI(aq) and NaOH

Ag+ or Pb2+ as a chloride (white ppt)

Fe2+ and Fe3+ and Al3+ as Fe(OH)2 (green/brown), Fe(OH)3
and Al(OH)3 (gelatine like)
Cu2+ as CuI2 (tan). Ni2+ as Ni(OH)2 (green).

III

Procedure
In your lab book, setup three columns as outlined below. Write potential equations whenever
there is a precipitate!!
Sample three column method:
Procedure
1. Added 3 drops 6 M HCl to
the known solution

Observation
A white ppt formed

2. Centrifuge the mixture

3. Decant supernatent

Solid settled to the bottom

Yellow supernatent

Conclusion and equations

Ag+ probably present
HCl(aq) + Ag+(aq) AgCl (s) + H+(aq)

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Okay, you are ready to start (as long as your lab book is setup).
First, you will test a solution of known ions, which are: Pb2+, Ag+, Fe2+ and 3+, Al3+, Cu2+, and
Ni2+.

Analysis of cations

I. Separation and detection of Ag+ and Pb2+.

Obtain a small test tube and place ten-15 drops of the known solution into it. Place 3 drops of 6
M HCl into the solution and mix. If a precipitate forms, centrifuge the mixture. Pour off the
supernatent liquid into a labeled test tube, and keep it for step 2. Wash the precipitate with five
drops of deionized water, and confirm the presence of Ag+ and/or Pb2+ with the confirming test.
Confirming tests:
For Pb2+: Add ~20 drops of distilled water to the ppt from above and put the test tube in a hot
water bath for 1 minute. Mix and while still hot, centrifuge. Decant the supernatant and keep
both supernatant and ppt. To the supernatant, add 2-3 drops of 1M K2CrO4. The formation of a
yellow ppt indicates Pb ions.
For Ag+: Add five drops of NH3(aq) to the precipitate from the Pb confirmation test. Mix the
mixture to break up the solid. Heat the test tube in a hot water bath. This should dissolve some
of the solid. Add 6 M HNO3 to the solution until it is acidic (red litmus stays red). If a white ppt
forms, Ag+ is present in the form of AgCl.
II. Separation and detection of Fe2+ and Fe3+ and Al3+.
Add five or six drops of ammonia (NH3 or NH4OH) to the solution and mix. Using a glass rod or
pipette, test the pH of the solution to determine if it is basic (red paper turns blue). If it is not
basic, add ammonia dropwise with mixing until it is basic. If a gelatin like substance is detected,
then aluminum is present. Look carefully for this here. It will be brown if there is iron and
aluminum ions, and white or clearish with just aluminum ion. Centrifuge the mixture, and decant
the supernatent liquid. Label the supernatant JIM. Keep this for step 3. Wash the ppt with 5
drops of water, and test it with the following confirming test.
Confirming test: Perform this only if there was a ppt in the last step. TEST the PPT.
A: To the solid ppt from step 2, add 8 drops of 6M NaOH. Stir the mixture, breaking up the
solid. Heat the test tube in a hot water bath. Centrifuge the solution. Decant, keeping both the
ppt and the supernatent liquid.
Test on the ppt from A above:
Add 10 drops of 6M HCl. Mix the mixture. The ppt will dissolve to form a light yellow solution.
Put a few drops of the solution into two wells of a well plate. To the first well, add 1 drop of
KSCN. A red solution proves Fe3+ is present. To the second well, add 2 drops of K4Fe(CN)6
solution. A dark blue confirms the presence of Fe2+.
Test on the supernatent liquid (from A, above, NOT the supernatent from step II (not JIM):
Add drops of 6M HCl until the solution is acidic (red litmus stays red). Add one drop of
aluminon reagent. Add drops of ammonia until the solution is basic. Stir and allow the solution
to stand. The formation of a red ppt proves that Al3+ is present.
III. Separation of Cu2+ and Ni2+.
To the supernatant JIM from test 2, add dilute HCl until the solution is just acidic. Add three
drops of potassium iodide and mix. A brown color will form, along with a tan ppt if copper ions
are present. Centrifuge and add one more drop of KI to see if more ppt develops. Repeat until no
more ppt forms upon addition of KI. Centrifuge and decant. Keep and label both!

Analysis of cations

Confirming test for Cu2+.

To the ppt: Wash once with water. Add 3 drops NH3 and then 2 drops H2O2. Mix. A deep blue
solution indicates Cu ions.
For Nickel: To the supernatant from part 3: If there is a brown color, add 2 drops of sodium
sulfate. Add 10-15 drops of NaOH. The solution needs to be really basic, pH>10. If a green ppt
forms, Ni ions are present.
Analysis of an Unknown
Obtain an alloy from the instructor. In the fume hood, dissolve the alloy in enough 12 M HNO3
to cover the sample, about 10 ml. Once it has completely dissolved, carefully add ~25 ml of
distilled water. Go through the entire procedure again, determining which ions are present. Not
all the ions will be present! If you do not get a ppt, that means that the ions are not there, so DO
NOT do confirming tests. The second run through should go much faster than the first.
Results Include a small results section indicating unknown # and ions found.
Ideas for the discussion/research.

Consider sources of error. Be specific. If you had troubles with a section, think hard
about why, and give some educated guesses about what happened.

Discuss how you know what your unknown ions are. Be specific and descriptive.
Compare the unknown results with what happened in the unknown. I do not want to have
to read all of your procedure/data to figure out what you did. What alloy did you have?

Have equations in your results area for ppt reactions that occurred. Highlight them so
they are easy to see.

Consider something from the list below. Research, cite sources. Connect this to our lives
and class.
What roles do these ions play in our lives? Why is detecting them important? When is
qualitative analysis used? What are these ions used for? Are they harmful? Helpful? Are
they in cereal? How are alloys made? What are they used for? What is solder and why are
there so many different kinds? Anything else that is related to the lab