Sneha Kannoth Mr.

Franz Organic and Biochemistry H February 6, 2012 Lab: Caffeine Distillation Objective: The purpose is to extract caffeine from a varied composition of tea leaves. Materials: Distilled water Beakers Tea Leaves [10-12 grams] Sodium Chloride [23 grams per each 100 m of combined extracts] Calcium Hydroxide [1 gram] Coffee filters Beuchner funnels Separatory funnel 2-propanol [25 ml] 10% aqueous NaOH solution [25 ml] Round Bottom flask [250 ml] Boiling chips Ice cubes [for ice bath] Heated water [for hot water bath] Stirring rod

Procedure: 1. Heat 200.0 mL of distilled water in a beaker, to boiling. 2. Heat 100.0 mL of distilled water in a beaker, to boiling. 3. After the 200.0 mL of distilled water has reached boiling, turn off the heat. 4. Add 10-12 grams of tea leaves to the 200 ml distilled water beaker. 5. Allow the tea leaves to spread within the distilled water solution for ten minutes. 6. Decant tea solution and press water out of tea leaves.

7. Allow the extracted solution to cool. 8. Place 25 ml of hot distilled water in the tea leaves. 9. Let it rest for five minutes. 10. Decant again and press out water. 11. Repeat process for a total of three times. 12. Filter final washing to gain all extract. 13. Join the washings with the initially extracted solution. 14. Add 23 grams of sodium chloride each 100 ml of combined extracted and 1 gram total of calcium hydroxide. 15. Heat solution for 15 minutes. 16. While heating, make certain to stir with stirring rod. 17. With coffee filters in the Beuchner funnels, recover remaining extract. 18. Transfer combined extract into separatory funnel. 19. Extract with 25 mL portions of 2-propanol. 20. Repeat three more times for a total of four successive 25 ml portions of 2-propanol. 21. Vent separatory funnel frequently, during initial mixing. 22. Before separating, make certain emulsion layer is not distinguishable. 23. Combine the 2 propanol extracts in a separatory funnel. 24. Wash once with 25 ml of 10 % NaOH (aqueous) solution. 25. Transfer 2-propanol solution into a 250 ml round bottom flask. 26. Add boiling chips. 27. Place stopper on round bottom flask. 28. Place flask in water bath. 29. Distill the 2 propanol from the caffeine extract using a water bath. 30. Monitor the temperature so that 2-propanol is distilled. Make certain that the water bath is not boiling out of control, otherwise the apparatus may explode and cause inaccurate results. 31. Approximately 15% of the total volume will be water that will remain after the 2propanol has been distilled. 32. Stop the distillation. Remove the round bottom flask w=from the hot water bath when no more distillate is being collected in the receiving flask. [the receiving flask is positioned to receive distillate as the round bottom flask is in hot water bath] 33. Take distilled 2-propanol product. 34. Measure volume.

35. Take remaining liquor; pour the liquor from a round bottom flask into a beaker, and allow it to cool. 36. Once room temperature, place it in an ice bath. [get a beaker, place many ice cubes in it, and allow the beaker to be engulfed within the ice cubes] 37. Ice baths will cause crystal formation. 38. Once crystal formation is complete, collect caffeine crystals using vacuum filtration. 39. Pre-weigh filter paper. 40. Dry caffeine product and measure mass. Observations: 1. The boiling chips certainly added stability to the process of distilling 2-propanol from the caffeine extract. Initially, we did not add boiling chips, and thus the hot water bath began to boil out of control, thereby causing us to continually reduce the temperature. The boiling chips added stability, and allowed us to maintain a moderate heated temperature, while collecting a good amount of distillate. 2. Once solution was heated for 15 minutes [in accordance with step 15], the solution of tea leaves had transformed into a murky, brown solution. It appeared to look as a cup of coffee, as it was a uniform color of muddy brown. It was also of a creamy texture, as there were certainly large particles of tea leaves still present in the solution. 3. When we had placed the remaining liquor into the ice bath, the liquor did not crystallize. The only event that occurred was that the liquor dropped to a lower temperature, yet there was no evidence of crystallization. Yet, I wonder if we had let it remain in the ice bath for another week, would crystallization have formed? For instance, was it simply a matter of time? Results: 1. We did not receive any results as our experiment had been properly conducted. In an attempt to crystallize the remaining liquor, we were not able to form crystallization. Thus, we received no mass of the caffeine crystals.