User:Paul Rothenberg/Notebook/Pauls Notebook/2013/05/29

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Reaction of OPD and H2O2 in Water with an Mb/Phosphate Catalyst

  • Objectives:
  • 1. Continue analysis of reaction of OPD+H2O2 with Mb/Phosphate catalyst
  • 2. Continue synthesis of Na12P2W18O62
  • Procedure for Part 1:
  • 1. Follow same protocol from 5/20 using Mb in Phosphate buffer with H2O as the solvent

The Mb did not dissolve in the same fashion as yesterday, when it went into water without vortexing. The solution was centrifuged

  • Data:

  • Observations
  • Even though the Mb did not dissolve in water even after centrifugation, there was still a reaction present at higher temperatures. The reaction at 15°C showed a peak between 350-375 nm, which disappeared following the course of the reaction. The reaction at 5°C did not, however, seem to react because of no definite peak at 460 nm; a peak between 350-375 nm was also seen in the final absorbance.

Synthesis of Na12P2W18O62

  • Procedure for Part 2:
  • 1. After the solution was left to reflux overnight, it was cooled and 100g of KCl was added
  • 2. Following the addition of KCl, the solution was filtered and the solid was placed in a massed beaker
  • 3. 200 mL of water was brought to 80°C, and 2x25 mL increments of water were added to the solid until it dissolved (for a total of 50 mL of hot water added)
  • 4. The mixture was placed in the fridge at 5°C to recrystallize overnight

The protocol for this reaction can be found here.

  • References:
  • 1. Finke et al, Trivalent Heteropolytungstate Derivatives, Journal of Inorganic Chemistry, 1987, 26, 3886-3896.