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The Synthesis of Alum

Mike Galdamez
5B
October 18, 2013

OBJECTIVES
In this experiment, a sample of alum will be synthesized. The process of creation will be
observed and recorded in order to calculate the percent yield of your synthesis.

MATERIALS
250 mL beaker
25 mL or 50 mL graduated cylinder
Bchner funnel and filter flask
watch glass
glass stirring rod
lab burner, ring stand, ring, wire gauze
plastic wrap or Parafilm
fume hood
hot plate

aluminum foil
3 M sulfuric acid solution, H2SO4
baking soda, NaHCO3
3 M potassium hydroxide solution, KOH
aqueous ethanol solution, 50%
vinegar, dilute CH3COOH solution
ice bath
balance

PROCEDURE
1. Obtain and wear goggles.
2. Obtain a piece of aluminum foil and measure its mass. For best results, you should have
about 1.00 g of aluminum. Tear the foil into small pieces and place the pieces in a 250 mL
beaker.
3. Set up a Bchner funnel and filter flask so that you are ready to filter the reaction mixture
that will be produced in Step 4.
4. Conduct the first part of the synthesis. CAUTION: Potassium hydroxide solution is caustic.
Avoid spilling it on your skin or clothing.
a. Use a graduated cylinder to measure out 25 mL of 3 M KOH solution.
b. Slowly add the KOH solution to the beaker of aluminum pieces. Notice that the reaction is
exothermic. Allow the reaction to proceed until all of the foil is dissolved.
c. Carefully pour the reaction mixture through your Bchner funnel and filter flask setup,
and rinse the filter paper with a small amount of distilled water. Note: The reaction
mixture contains three ions: K+, [Al(OH)4], and excess OH.
d. Rinse the beaker with distilled water, and pour the filtered liquid back into the beaker.
5. Allow the solution to cool to near room temperature. If you are pressed for time, you may
cover the beaker with plastic wrap or Parafilm, and store the liquid overnight.
6. Clean the Bchner funnel and filter flask, and prepare it for more filtering that you may need
to do in Step 7 or Step 10.

7. Complete the synthesis.


a. Use a graduated cylinder to measure out 35 mL of 3 M H2SO4 solution. CAUTION: The
reaction mixture must be cooled to room temperature before proceeding. Handle the
H2SO4 solution with care. It can cause painful burns if it comes in contact with the skin.
b. After the reaction mixture has cooled, slowly add the sulfuric acid solution to the beaker
of liquid. Stir the mixture constantly. The reaction is strongly exothermic, so be careful as
you stir the mixture. Note that aluminum hydroxide will precipitate initially. It will
dissolve as more sulfuric acid is added.
c. If there is some solid remaining in the beaker after the 35 mL of sulfuric acid has been
added, pour the mixture through the Bchner funnel and filter flask to separate the
undissolved solid from the mixture.
8. Gently boil your mixture until you have about 50 mL of liquid in the beaker.
9. Cool the beaker of solution. Choose one of the two methods listed below.
Allow the solution to cool overnight. In most cases, this gradual cooling forms a good
crop of alum crystals.
Prepare an ice bath for the 250 mL beaker. Place your beaker of solution, uncovered, in
the ice bath. Do not move the ice bath or the beaker. After about fifteen minutes, crystals
of alum will appear in the beaker. If there are no crystals after fifteen minutes, scrape the
bottom of the beaker with a glass stirring rod to create a rough spot for crystal growth.
You may also heat the solution to evaporate more water and cool the solution again.

10. Collect your alum crystals by pouring them onto the Bchner funnel and filter-flask setup.
Use vacuum filtration to wash the crystals on the filter paper with 50 mL of an aqueous
ethanol solution (50%). The crystals will not dissolve in this solution.
11. Remove the filter and crystals from the Bchner funnel and allow the crystals to dry at room
temperature. Measure and record the mass of your sample of alum. Store the crystals for
further analysis.

DATA

Mass of Aluminum (g)

.0987

Mass of empty watch glass (g)

53.318

Mass of watch with crystals (g)

68.591

Mass of Crystals (g)

15.273

OBSERVATIONS

As KOH is added to the Al, the dissolving of the Al creates a white gas, which is the H2
being created from the reaction. That caused the reaction to bubble. The solution also
changed from clear to dark grey. Since the reaction was exothermic, the given off could
be felt. As the solution is filtered the color becomes a clear solution, from the filtering
of any impurities that may have given the original dark-grey pigment.

As H2SO4 is poured into the solution, a white precipitate was formed as solid Al (OH) 3.
The precipitate is later filtered out and the solutions color goes back to clear instead of
a cloudy white.
Later on once crystals formed, it can be seen that our crystals were very small and
taking up the bottom completely. They were hard to remove at first, was made easier
with the help of the ethanol solution.

DATA ANALYSIS
1.

Determine the theoretical yield of the alum. Use the aluminum foil as the limiting
reagent and presume that the foil was pure aluminum.
.987g Al

.0366 mol Al

1mol Al
26.98g Al

= .0366 mol Al

1 mol Alum
1 mol Al

474.39 g Alum
1mol Alum

Alum

= 17.365g

Theoretical Yield is 17.365g of Alum


2.

Calculate the percent yield of your alum crystals.


(15.273g Alum/17.362g Alum)*100 = 87.97%

3.

Discuss the factors that affected the percent yield.


One of the factors that affected our percent yield was the loss of alum crystals while
trying to remove them from the filter paper. The crystals were very small and hard to
unstick from the paper. When scraping the paper, some crystals flew off which
affected our mass. During the transfer from funnel to watch glass, some of our
crystals may have been lost again due to size.

4.

Write the balanced net ionic equations for the following: (a) aluminum and potassium
hydroxide, yielding [Al(OH)4] and hydrogen gas; (b) hydrogen ions and [Al(OH)4] ,
yielding aluminum hydroxide; (c) aluminum hydroxide and hydrogen ions, yielding
[Al(H2O)6]3+; and (d) the formation of alum from potassium ions, sulfate ions, []3+,
and water.
A: 2 Al(s) + 2 OH-(aq) + 6 H2O(liq) 2 Al(OH)4-(aq) + 3 H2(g)
B: Al(OH)4-(aq) + H+(aq) Al(OH)3(s) + H2O(liq)
C: Al(OH)3(s) + 3 H (aq) Al (aq) + 3 H2O(liq)
D: K (aq) + (Al(H2O)6) (aq) + 2 SO4 (aq) + 6 H2O(liq) KAl(SO4)212 H2O(s)
+

5.

3+

3+

2-

Describe a synthesis reaction.


A synthesis is a type of chemical reaction in which two or more simple substances
combine to form a more complex product. The reactants may be elements or
compounds. The product is always a compound. An Example is when Aluminum
combined with Potassium hydroxide and water to form KAL(OH)4 and 3H2.

6.

Describe how the solubility of alum in various solvents and water at different
temperatures was used in conducting the experiment.
The temperature of the solvents will determine how long the alum will take to
dissolve. The higher the temperature of the solvent is, the less time it will take to
dissolve.

7.

Write a detailed description of the alum crystals.


The alum crystals formed based around a specific shape, the triangle. When you look
closely at the alum crystals, you will see that their shape is basically overlapping
triangles. This caused the crystals to appear with many ridges round the outside. Most
of the crystals we obtained were extremely small and only one was actually big
enough to see the previously described features. Our crystal also appear to be cloudy
and white. The cloudiness was actually small crystals sticking to the larger one.

CONCLUSION:
The main purpose of this experiment was to synthesize alum and see how we did it.
After seeing our percent yield, it can be seen that we had some errors; 13.03% to be
exact. The amount of errors was most likely caused by the size of our crystals. Our
beaker had many imperfections at the bottom which caused many small crystals to
form all around the bottom. When transferring the small crystals at any time, we
always lost some. I believe that if we had a newer beaker our percentage error would
be much smaller.