User:Paul Rothenberg/Notebook/Pauls Notebook/2012/09/19

19 September 2012

• Procedure for 19 September 2012':

• 1. Amounts of Nickelous Sulfate and Protoporphyrin IX were measured out based on Stoichiometry (1).
• 2. 46 mg (44.2 mg) of Nickelous Sulfate and 100 mg (100.5 mg) Protoporphyrin IX were measured out on a balance.
• 3. 10 mL DMF is added to a 50 mL round-bottom flask with a 19/22 Opening (1)
• 4. The flask was placed on a heating pad with a 100 Volt Volt-ac with a stir bar under the presence of Nitrogen.
• 5. The DMF was brought to reflux under these conditions (1).
• 6. Once the DMF was in reflux, the protoporphyrin IX was added, and let reflux (1).
• 7. The Nickelous Sulfate was then added, and let reflux for 30 minutes (1).
• 8. The flask was then chilled in an ice bath for 15 minutes (1).
• 9. 100 mL of chilled water was then added, was left to chill for 10 minutes, and the precipitate is filtered using a Buchner funnel (1).
• 10. The filtered material was washed with water (1).

• See Dr. Harting's notebook for the filtration results.

• References:

1. Adler, Alan D. On the preparation of metalloporphyrins. Journal of Inorganic Nuclear Chemistry, Vol.32. 1970.