User:Paul Rothenberg/Notebook/Pauls Notebook/2012/09/19: Difference between revisions
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*Procedure for 19 September 2012': | *Procedure for 19 September 2012': | ||
1. Amounts of Nickelous Sulfate and Protoporphyrin IX were measured out based on Stoichiometry (1). | *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. | *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) | *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. | *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). | *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). | *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). | *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). | *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). | *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). | *10. The filtered material was washed with water (1). | ||
*See Dr. Harting's notebook for the filtration results. | *See Dr. Harting's notebook for the filtration results. |
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19 September 2012
1. Adler, Alan D. On the preparation of metalloporphyrins. Journal of Inorganic Nuclear Chemistry, Vol.32. 1970.
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