Synthesis of Alum (Calculating Theoretical And Percent Yield)

October 10, 12, 14, 2011

Andy Nguyen

2=complete 1=partial 0=not at all Design (D) Data Collect. & Proc (DCP) | | Conclusio n & Eval (CE) | |

Synthesis of Alum (Chemical Recycling of Al)

Scrap (2005)

(This handout has been adapted from John Kotzs experiment entitled, The Synthesis of Potassium Aluminum Sulfate (Alum) From Aluminum

Introduction: In this experiment the ionic compound, potassium aluminum sulfate (KAl(SO4)212H2O), will be prepared from a water solution that contains K+, Al3+, and SO42- ions. The aluminum ions will be formed by oxidizing aluminum metal from a soda can. The double salt potassium aluminum sulfate dodecahydrate is commonly referred to as alum. Many combinations of mono- and tripositive cations yield crystals of the same stoichiometry and structure, and alum is a general name for this type of compound. Alums have a wide range of uses. Potassium alum is used in cosmetics such as a deodorant and aftershaves. Sodium alum is used in the canning of garden vegetables (although not as commonly today as it causes gastric pain in some individuals) and in the preparation of baking powder. If an aqueous solution which contains [Al(H2O)6]3+ ions, K+ ions and SO42- ions is allowed to evaporate, the compound KAl(SO4)212H2O will crystallize. Aluminum is considered a reactive metal, but because its surface is usually protected by a thin film of aluminum oxide, it reacts only slowly with acids. It does, however, dissolve quickly in basic solutions. Excess hydroxide ion converts the aluminum to the tetrahydroxoaluminate (III) ion, [Al(OH)4]- : Al (s) + KOH (aq) + H2O (l) K[Al(OH)4] (aq) + H2 (g) When acid is slowly added to this ion, white, gelatinous aluminum hydroxide, AIOH)3, precipitates: K[Al(OH)4] (aq) + H2SO4 (aq) Al(OH)3 (s) + H2O (l) + K2SO4 (aq) Continued addition of acid causes the precipitate of Al(OH)3 to dissolve as it is neutralized by the sulfuric acid: Al(OH)3 (s) + H2SO4 (aq) Al2(SO4)3 (aq) + H2O (l) The solution at this point contains Al3+ ions, K+ ions, and SO42- ions. Upon cooling, crystals of hydrated potassium aluminum sulfate KAl(SO4)212H2O (or alum) are very slowly deposited: Al2(SO4)3 (aq) +K2SO4 (aq) + H2O (l) KAl(SO4)2 12H2O (s)

Materials: distilled water 50 mL 1.4 moldm-3 KOH 20 mL 9 moldm-3 H2SO4 50 mL 50% ethanol/water aluminum can ice scissors steel wool 125 mL Erlenmeyer flask glass stirring rod 10 mL graduated cylinder Procedure: DAY 1: 1. Clean all glassware.

electronic balance 250 mL beaker 600 mL beaker ring stand iron ring with wire gauze Bunsen burner with tubing flint striker filter paper x 2 funnel Bchner funnel apparatus 100 mL graduated cylinder

2. Pierce an aluminum can at the lower end of the side with the point of a pair of scissors. Carefully cut around so that the sides of the can are cut out. Deposit the waste aluminum scraps left over in the box provided by your teacher. 3. Lay the rectangular piece of aluminum (the sides of the can) on the bench and scour both sides with a piece of steel wool. Make sure that an area of 6 cm x 6 cm is clean on both sides. 4. Take aluminum to the analytical balance and mass it. If the piece weighs more than 1 g, cut small pieces off until it weighs just under 1 gram. Now weigh the piece of aluminum precisely and record the mass in your data table. 5. Cut the weighed piece into smaller pieces and place them in a clean 250 mL beaker. 6. DO THIS NEXT STEP IN THE FUME HOOD: Using a graduated cylinder, add 50 mL of 1.4 moldm-3 KOH. 7. Set up a ring stand, iron ring, gauze, and Bunsen burner. Place the beaker on the gauze and heat the beaker on a low flame. It is not necessary to boil it. The aluminum will take anywhere from 10-20 minutes to dissolve (be careful to not let the solution boil over).

8. While it is dissolving, set up an apparatus for gravity filtration. Place a clean funnel, with a piece of folded filter paper, on a 125 mL Erlenmeyer flask. 9. When the aluminum has dissolved (as evidenced by the lack of bubbles of H2 gas given off), gravity filter the solution. Only fill the funnel to within inch of the top of the paper. Use a glass stirring rod to guide the solution into the paper. The solution in the Erlenmeyer flask should be both clear and colorless at this point. 10. Allow the flask to cool. While it is cooling, wash the funnel and beaker with tap water to remove any potassium hydroxide. 11. When the solution is reasonably cool, add 20 mL of 9 moldm-3 H2SO4 (under the supervision of your teacher) quickly and with care. It is important that you swirl the flask as you add the acid. The solution will get quite warm. If there are any white flecks left in the solution after the addition of the H2SO4, place the flask on the Bunsen burner apparatus and warm it with swirling until all of the solid material has dissolved. 12. When the flask has cooled sufficiently to pick up, label with tape identifying your group and place in an area designated by your teacher until Day 2 of the experiment (alum crystals will form overnight). DAY 2: 13. Make an ice bath by putting ice and water into a 400 mL beaker. Using a graduated cylinder, measure 50 mL of 50% ethanol/water mixture and place into a large test tube. Place the test tube containing the 50% ethanol/water into the ice bath. 14. Set up a vacuum filtration apparatus (Bchner funnel) as illustrated by your instructor. Record the mass of your dry filter paper. Pour some distilled water onto the filter to seal it to the funnel. 15. Take the flask containing the alum crystals and swirl so that all the crystals are dislodged. Quickly pour the solution containing your alum crystals into the Bchner funnel. Keep swirling and pouring until all the solution and crystals are transferred to the funnel. The water aspirator should be kept going all through this process. 16. Pour about 10 mL of the cooled alcohol/water mixture into the flask. Swirl the flask and pour the mixture into the funnel to transfer any remaining crystals. 17. Wash the alum crystals, now on the filter, with the cool alcohol/water mixture using the following procedure: Disconnect the aspirator hose from the aspirator unit on the faucet. Pour about 5-10 mL of alcohol/water onto the crystals and gently stir. Reconnect the aspirator hose, and allow the crystals to dry for about 3 minutes. 18. Place the nearly dry alum crystals in the evaporating dish in a cupboard specified by your teacher until the next lab period.

DAY 3: 19. Precisely weigh your yield of crystals + filter paper. 20. Dispose of your alum crystals in the container specified by your teacher. Data Collection: Aluminum = 0.7873 (+/- 0.0001g) Dry Filter Paper = 0.5224 (+/- 0.0001g) Crystal + Filter Paper = 5.0053 (+/- 0.0001g) Qualitative Observations: When 50 mL of 1.4 moldm-3 KOH was added into a beaker filled 0.7873 g of aluminum, the mixture started to bubble. After placing the beaker on a heat source (the Bunsen burner) and letting it heat up for a while, the mixture began turning grey and soon into black after approximately 10 minutes. After filtering the mixture, the liquid became clear and colorless. 20 mL of 9 4 moldm-3 of H2SO4 was added into the solution, creating white material. The white material was dissolved after heating on the Bunsen burner. Once the crystals were rinsed with 50% ethanol/water solution and left to dry, the crystals began to look like sugar. Data Analysis: 1. Balance each of the separate chemical equations shown in the introduction. 2. Combine the separate balanced equations into 1 reduced chemical equation. 3. Use stoichiometry to determine your theoretical yield of alum (assuming the Al metal is the limiting reactant). Be sure to show your work (factor label). 4. Calculate the percentage yield of your alum.