Preparation of ALUM

Purpose
In this experiment you will synthesize potassium sulfate dodecahydrate (alum), isolate the product
and calculate percent yield.
Introduction
Alums are ionic compounds that crystallize from solutions containing sulfate ion, a trivalent cation
such as Al3+, Cr3+, or Fe3+ and a monovalent cation such as K+, Na+, or NH4+. Six of the water
molecules bind tightly to the trivalent metal ion; the remaining six molecules bind more loosely to
the monovalent cation and the sulfate anion.

Alum crystals of great purity are easily prepared. Because of this purity, alum is useful in the
dyeing of cloth, where the alum acts as a source of A13+ ions which are not contaminated with
Fe3+. The A13+ is precipitated on the cloth as aluminum hydroxide which acts as a binding agent
for dyes. It is necessary that no Fe3+ be present to produce clear colors.

In this experiment, you will synthesize alum and calculate the theoretical, experimental, and
percent yields.

An alum is a hydrated double sulfate salt. The alum which you will prepare is potassium aluminum
sulfate dodecahydrate, or potassium alum, and has the formula KAl(SO4)2•12H2O. Your starting
material for this synthesis will be an aluminum beverage can.

The pieces of aluminum metal is first dissolved and oxidized by a hot potassium hydroxide solution:
2Al(s) + 2KOH (aq) + 6H2O(l) → 2 KAl(OH)4 (aq) + 3H2(g)

After filtration to remove any residual impurities from the original aluminum sample the solution
should be clear and colorless. Then sulfuric acid is added to the reaction mixture and two sequential
reactions occur. Initially, as the acid is added a precipitate aluminum hydroxide forms.
2 KAl(OH)4 (aq) + H2SO4 (aq) → 2 Al(OH)3(s) + K2SO4 (aq) + 2H2O(l)

Then as more sulfuric acid is added with heat the aluminum hydroxide precipitate dissolves.
2 Al(OH)3(s) + 3 H2SO4 (aq) → Al2(SO4)3 (aq) + 6H2O(l)

This leaves aluminum ions in solution. The solution at this point also contains potassium and sulfate
ions. On cooling these ions the alum crystalizes out of solution.
Al2(SO4)3 (aq) + K2SO4 (aq) + 24 H2O(l) → 2 KAl(SO4)2•12H2O(s)

One of the interesting properties of aluminum is that it is amphoteric, meaning it will dissolve in
both strong, aqueous acids and strong, aqueous bases. In both cases, the formation of hydrogen
gas is observed

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 Equipment
• Aluminum starting material • Filter funnel and filter paper
• 6 M H2SO4 • Hot plate
• 4 M KOH • Buchner funnel, Side arm flask,
• 50/50 ethanol/water mixture vacuum hose
• Ethanol • Stirring rod/rubber policeman
• 250-mL beaker • Ice and a large beaker or tub for the
• 150-mL beaker ice bath
• 50-mL graduated cylinder

Safety Precautions
Be sure to wear safety goggles when you do this experiment. The concentrated sulfuric acid and
potassium hydroxide used in this lab are both highly damaging to skin and eyes. During the
dissolution of the aluminum foil, hydrogen gas is produced. This step should be performed in a
fume hood and no flames or heat sources should present in the area.

Experimental Procedure
1. Obtain ~1 gram of scrap aluminum in a 250-mL beaker and measure the exact mass of the
Al.

2. In the fume hood, slowly add 25 mL of 4 M KOH to the beaker containing the aluminum.
This step will produce fumes and heat, so proceed slowly and carefully. Stir the mixture with
a clean stirring rod until the reaction is complete.

3. If the reaction is slow or incomplete heat the mixture for 30 minutes in order to dissolve as
much of the aluminum as possible. Stir frequently to keep the metal pieces from floating to
the top. If necessary, add water to keep the volume constant (at ~25 mL).

4. Place a clean funnel in a funnel stand or an iron ring attached to a ring stand. Place a filter
paper into the funnel. To do this, take a piece of round filter paper fold it in half, then fold it
in half again. Open the filter paper up so that you have a cone shape. Put the filter paper in
the funnel and get it to stick in the funnel by wetting the paper with a stream of deionized
water from your wash bottle. This is called “seating” the filter paper in the funnel.

5. Place an empty 150-mL beaker under the funnel to collect the liquid filtrate. Gravity filter
your reaction mixture by pouring it through the filter paper in the funnel, being careful to not
fill the filter paper more than ¾ full at a time because the reaction mixture can creep up and
over the side of the filter paper.

6. Allow the clear filtrate solution collected in the 150-mL beaker to cool. Place the used filter
paper into the waste in the hood.

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7. Obtain about 20 mL of 6 M H2SO4 in a 50-mL graduated cylinder. Slowly add small
increments of the H2SO4 to the reaction solution while stirring. Continue adding small
increments until a white, insoluble solid (Al(OH)3) starts to form. This should occur after the
addition of ~15–18 mL of H2SO4.

8. Gently heat the solution while stirring until any solid Al(OH)3 has dissolved. At this point the
solution should be clear.

9. Create an ice bath by filling a large beaker or tub ½ to ¾ full with ice then add a small
amount of cold water. Cool the reaction solution in the ice bath for about 20–30 minutes, at
which point alum crystals should have formed. If no crystals are evident, reheat the solution
until the total volume has decreased to half the original volume (10–12 mL). Cool the
solution until ALUM crystals have formed.

10. Set up a vacuum filtration system fitted with an adapter and a Buchner funnel. Obtain a filter
paper to put into the top of the Buncher funnel.

11. Mass the top of the Buncher funnel and the dry filter paper.

12. Turn on the vacuum and wet the filter paper with a small amount of water, pushing down on
the funnel to obtain a better vacuum seal. Pour your suspension of crystals onto the filter
paper. Allow the liquid to drain completely, then wash out the beaker with 10 mL of 50/50
ethanol/water solution in order to completely transfer any crystals still left in it. Pour this
mixture (in which the alum is not very soluble) over the crystals in the funnel and again let
the liquid drain.

13. Finally, wash the crystals with 10 mL of ethanol. Leave the vacuum on for about 5 minutes
in order to draw air through the crystals to dry them.

14. Remove the top of the Buchner funnel (with the filter paper and alum crystals) and place this
in your drawer to dry until the next lab period.

15. Dispose of all filtrate liquid into the waste bottle in the hood.

Cleanup: All liquid filtrate should be disposed of in the waste container in the hood. The filter
paper form the gravity filtration step should be disposed of in the solids waste in the hood. Return
the DI bottle that you used to its proper place. Clean all equipment that you used, dry them with
a paper towel, and return them to their proper storage drawers. Clean your lab bench work
space with a wet paper towel.

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Name: __________________________

Preparation of ALUM: Pre-lab Questions

1. Be sure that you arrive to lab on time, bring your lab goggles to lab and come properly dressed.
Read through the experiment and set-up your notebook BEFORE you come into lab (Title,
Date, Purpose, Safety, Equipment List, Overview of Procedure and Data Tables).

2. Calculate the molar mass of potassium aluminum sulfate dodecahydrate, KAl(SO4)2 •12H2O.
Be sure to include the twelve waters of hydration in the molar mass.

3. Why should you NOT wash the crystals with pure water?

4. Write out the net ionic reactions for each of the four reaction steps given in the introduction.

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Name: __________________________ Notebook Grade: __/5_

Preparation of ALUM: Report Sheet

Mass of Al starting material (g)

Mass of Buchner funnel top and filter paper (g)

Mass of Buchner funnel top, filter paper and ALUM (g)

1. Which reactant is the limiting reactant in this synthesis? Prove your answer by showing the
calculations of how many moles of each reactant is added in each of the four reaction steps
shown in the Introduction.

2. Determine the theoretical yield, in grams, of the ALUM crystals.

3. Calculate the percent yield of your ALUM crystals.

4. Give one reason why your percent yield could be >100% and one reason why your percent
yield could be <100%.