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Synthesis of Alum: KAl(SO4)2 12H2O

Purpose:
The purpose of this lab is to synthesize a specific type of alum from aluminum foil and
various chemicals through a series of chemical reactions.
Materials/Safety:
1. Chemicals

Aluminum foil

Sulfuric Acid, H2SO4, 3M

Baking Soda, NaHCO3

Potassium Hydroxide, KOH, 3M

Water-Ethanol solution, 50% by volume

Vinegar, dilute HC2H3O2

2. Equipment

Beaker, 250 mL

Graduated cylinder

Bchner funnel and filter flask

Ice bath

Balance

Watch glass

Stirring rod

Burner, ring stand, ring, wire gauze

Plastic wrap or Parafilm

Fume Hood

3. Safety

If any acid or base is spilled, wash off with lots of water.

Due to high concentrations of sulfuric acid and potassium hydroxide, the use of
chemical splash goggles and a chemical resistant apron is necessary.

Neutralize sulfuric acid spills with baking soda

Neutralize potassium hydroxide spills with vinegar

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When dissolving aluminum in potassium hydroxide solution, hydrogen gas is
produced. Make sure there are no flames nearby and that this step is performed in
a fume hood.
Procedure:
1. Weigh Out and Dissolve the Aluminum

Weigh out about 1 gram of aluminum foil to the nearest centigram. Tear the foil
into small pieces and place in a 250 mL beaker.

SLOWLY add 25 mL of a 3M KOH solution. Allow the reaction to proceed until

all of the foil is dissolved. Remove any undissolved solids such as carbon
particles by filtering the solution through a Bchner funnel while the solution is
hot. Rinse the filter paper with a small amount of distilled water.

2. Acidify with Sulfuric Acid

At this point the solution contains [Al(OH)] and K ions. Cool the solution and
then acidify it slowly, with constant stirring, using 35 mL of 3M HSO. The
solution will get very hot because you are adding strong acid to the strongly basic
solution. Solid Al(OH) will first precipitate and then dissolve as more HSO is
added. If a precipitate still remains, filter the solution and discard the solids. You
can use vacuum filtration with a Buchner funnel and filter flask to speed up this
process. Then boil the solution until water has evaporated to give a volume of
about 50 mL of solution. This is a good place to stop if the end of the lab period
is near. Cool the solution and cover the beaker with Parafilm or plastic wrap.
Allow it to rest undisturbed until the next period.

3. Crystallize the Alum

If time permits, cool the solution in an ice bath for 15 minutes, keeping it as
motionless as possible. Crystals of alum should grow in the beaker. If no crystals
form, scrape the bottom of the beaker with a stirring rod to create a rough place
where crystals may begin to grow, or add a seed crystal. If there are still no
crystals, reheat the solution until more water has evaporated and then cool again.
Rapid cooling in an ice bath causes very small crystals to grow; slow overnight
cooling allows the formation of larger crystals. (We did not execute these

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particular steps in our experiment.) Collect the alum crystals by vacuum filtration.
We then washed the crystals with 50 mL of a 50% by volume water and ethanol
mixture, in which alum crystals are not very soluble. Allow the crystals to dry at
room temperature. Determine the mass of the alum. Calculate the theoretical
yield of alum assuming that aluminum was the limiting reactant and that the foil
was 100% aluminum, and calculate your percent yield.
Data:
Mass of Wax Paper

0.39g

Mass of Wax Paper w/ Aluminum

1.19g

Mass of Aluminum

0.80g

Mass of Ziploc Bag

6.33g

Mass of Ziploc Bag w/ Alum Crystals

14.15g

Mass of Alum Crystals

7.82g

Calculations:
Calculation 1: Mass of Wax Paper and Aluminum Foil - Mass of Wax Paper = Mass of
Aluminum Foil
1.19 g 0.39 g = 0.80 g
Calculation 2: Mass of Ziploc Bag w/ Alum Crystals - Mass of Ziploc Bag = Mass of
Alum Crystals
14.15 g 6.33 g = 7.82 g
Calculation 3: Theoretical Yield
K + Al +2SO + 12HO KAl(SO) 12Ho
K + Al +2SO + 12HO KAl(SO) 12HO
(0.80 g Al/1) * (1 mol Al/ 26.982 Al) * (1 mol Alum / 1 mol Al) * (474.338 g
Alum / 1 mol Alum) = 14.1 g Alum
Theoretical yield of alum=14.1 g Alum
Percent Yield
7.82 g / 14.1 g= 55.4%

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Result: 0.80g of aluminum produced 7.82 g of KAl(SO) 12HO which corresponds

to a 55.4% theoretical yield assuming at the aluminum was the limiting reactant and that
the foil was 100% aluminum.
Discussion Questions and Answers:
1. Write balanced net ionic equations for the following reactions which occur in this
synthesis:
a. Aluminum reacts with KOH and water forming potassium ions, and hydrogen
gas;
2Al (s) + 2KOH (aq) + 6H2O (l) 2K+ (aq) + 2[Al(OH)] + 3H2 (g)
2Al (s) + 2K+ (aq) + 2OH + 6H2O (l) 2K+ (aq) + 2[Al(OH)] + 3H2 (g)
2Al (s) + 2K+ (aq) + 2OH + 6H2O (l) 2K+ (aq) + 2[Al(OH)] + 3H2 (g)
2Al (s) + 2OH- + 6H2O (l) 2[Al(OH)] + 3H2 (g)
b. Hydrogen ions from the acid react with the tetrahydroxoaluminate ions to
precipitate aluminum hydroxide;
2K+ + H2SO4 (aq) + 2[Al(OH)4]- (aq) 2Al(OH)3 + 2H2O + K2SO4 (aq)
2K+ (aq) + 2H+ + SO42- (aq) + 2[Al(OH)4]- (aq) 2Al(OH)3 + 2H2O (l) + 2K+ (aq) + SO42- (aq)
2K+ (aq) + 2H+ + SO42- (aq) + 2[Al(OH)4]- (aq) 2Al(OH)3 + 2H2O (l) + 2K+ (aq) + SO42- (aq)

[Al(OH)4]- (aq) + H+ (aq) Al(OH)3 (s) + H2O (l)

c. Aluminum hydroxide reacts with additional hydrogen ions and water to form
[Al(HO)];
Al(OH)3 (aq)+ 3H+ (aq) + 3H2O (l) [Al(HO)] (aq)
d. Alum forms from the potassium ions, hydrated aluminum ions, sulfate ions and
water.
K+ + [Al(H2O)6]3+ + 2SO42- + 6H2O KAl(SO4)2 12H2O
2. What is a synthesis reaction?
A synthesis reaction is chemical reaction in which two or more simple substances
combine to form a more complex compound.

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3. Why should you NOT expect a 100% yield of crystals?

Dua

The aluminum foil could have not been 100% aluminum and the filtration process
could have not removed all impurities in the solution. Limiting reactants may not
be 100% pure.

3. How does the solubility of alum in water change with temperature?

As the temperature increases, the solubility increases proportionally. Conversely,

as the temperature decreases, the solubility of the alum decreases proportionally,
as well.

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

Water wouldve redissovled the crystals because dehydrating a solution of

aluminum, potassium, and sulfur formed them. Also, due to the polarity of water,
we used ethanol instead so the crystals would not dissolve.

3. What do your crystals look like?

Our crystals look like crushed, white glass. Each crystal within the product looked
almost identical and the product itself had a bright white color. We produced a
large quantity, as well.

3. What is the shape of an octahedron?

An octahedron is an eight-faced polyhedron consisting of 8 equilateral triangular

faces; it is a composition of 2 square pyramids.

3. Show how you obtained your theoretical and percent yields.

Theoretical Yield
K + Al +2SO + 12HO KAl(SO) 12HO

(0.80 g Al/1) * (1 mol Al/ 26.982 Al) * (1 mol Alum / 1 mol Al) * (474.338 g
Alum / 1 mol Alum) = 14.1 g Alum

Theoretical yield of alum=14.1 g Alum

Percent Yield

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7.82 g / 14.1 g = 55.4%

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