Lab #3 

 
A Synthesis Experiment: The Preparation of Alum
 
David Morales and Franica Brown 
January 24th, 2019 
 
 
 
 
 
 
 
 

For this experiment we will be using various measurement devices, lab equipment, and
chemicals to prepare potassium aluminum sulfate dodecahydrate (alum), from scrap metal.
Starting with an initial aluminum mass of 0.4199g, our theoretical yield of alum was calculated
to be 7.3827g. Due to a lack of drying time, our actual measured yield of alum was measured out
7.9283g, driving a percent yield of 107.39%. The class average percent yield was 83.89%, and
the standard deviation was 26.24%.

Procedure:
1. Obtain a piece of an aluminum can that weighs approx. ½ gram, use sand paper on the
outside and inside to remove paint and clear finish, respectively.
2. Cut an estimated .4 gram of the can into smaller pieces, weigh using the analytical
balance and record-be careful of sharp edges.
3. Add pieces to a 150 mL beaker, set up on a ring stand with an iron ring and wire gauze.
4. Add 10.0 mL of 3.0 M potassium hydroxide to the beaker-use caution and proper
protective gear when handling caustic chemicals.
5. Set a Bunsen burner under the beaker and heat the solution with a low flame.
 SMALL AMOUNTS OF HYDROGEN GAS WILL BE PRODUCED
DURING THE FOLLOWING STEPS. DO NOT ALLOW THE FLAME
OF THE BURNER TO REACH THE TOP OF THE BEAKER.
EXTINGUISH THE FLAME IF THE REACTION BECOMES TOO
VIGOROUS.
6. After the initial reaction, continue to gently heat the beaker until all the aluminum
dissolves.
7. Maintain 10 mL volume by adding distilled water as required.
8. Remove suspended particles of paint with spatula or stirring rod.
9. Remove from heat and allow to cool to room temperature, an ice bath may be used to
accelerate the process.
10. Slowing acidify the solution by adding 6M sulfuric acid in drops while stirring to a
volume of 10.0 mL acid solution added.
11. If there is still a solid present, stir and heat the solution, adding distilled water to maintain
22-23 mL total solution volume.
12. Remove beaker from heat, place on a porcelain stand and cool for 30 minutes to room
temperature and then an additional 15 minutes in an ice bath. Slow, undisturbed crystal
growth will result in larger, purer crystal.
13. Consult instructor if crystals do NOT form. Corrective actions in order of preference are:
add a seed crystal to initiate crystal growth, scratch the sides of the beaker with a un-fire
polished stirring rod, place beaker into ice bath again, reheat solution to evaporate some
water and allow to cool again.
14. After successful crystallization, collect the crystals by suction filtration using a Bucher
funnel and a side arm filter flask. The paper should just cover the holes on the bottom of
the Bucher funnel and should not come up the funnel. Wet the paper before turning on
the aspirator.
15. Transfer most of the crystals using the spatula, leaving some solution in the beaker to aid
transferring the smaller crystals. Rinse the beaker with a 50:50 mix of alcohol and water,
then use rinse solution to wash the crystals in the funnel.
16. Transfer the crystals to a labeled watch glass and dry in a 60° oven.
17. Calculate the theoretical yield of alum based on the initial mass of aluminum and
calculate percent yield.
 18. Record team initials on blackboard with percent yield. Record data on the board, this is
needed to calculate average percent yield and standard deviation for the class.

Post-Experiment Clean-Up

1. Excess potassium hydroxide should be neutralized with 6M sulfuric acid in drops until
the solution turns litmus paper red. Excess acid will cause bubbling; add sodium
bicarbonate until bubbles cease. Pour neutral solution slowly into sink with running
water.
2. Excess acid should be diluted by adding acid to water and neutralizing the resulting
solution with sodium bicarbonate.
3. Clean the filter paper by neutralizing with the sodium bicarbonate and disposing down
the sink as prescribed above.
4. Aluminum can scrapes can be returned to the aluminum container.