User:Paul Rothenberg/Notebook/Pauls Notebook/2012/09/26

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26 September 2012

  • The same reaction will be run as last week, except with 250 mg of Protoporyphrin IX and 115 mg of Nickelous Sulfate.
  • The same procedure will be followed.

  • 1. 250 mg Protoporyphrin IX and 115 mg Nickelous Sulfate was measured out on a balance
  • 2. 25 mL DMF is added to a 50mL Round-Bottom flask with a 19/22 opening
  • 3.. 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 DMF was brought to reflux under these conditions (1).
  • 5. Once the DMF was in reflux, the protoporphyrin IX was added, and let reflux (1).
  • 6. The Nickelous Sulfate was then added, and let reflux for 30 minutes (1).
  • 7. The flask was then chilled in an ice bath for 15 minutes (1).
  • 8. 250 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. Nylon filter paper was used to collect the crystals. The filter paper is massed to be 0.0708 grams.
  • 10. The mixture was run through a vacuum filtration setup.
  • 11. The mass of the filter paper plus compound is 1.1461g Edited by Matt Hartings

  • References:

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