User:Matt Hartings/Notebook/Photosynthesis/2013/06/21

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POM Synthesis

Today I'm performing the synthesis of K8HP2W15V3O62-9H2O following this protocol. The only difference is that I"m scaling the synthesis down by a factor of 10.

  1. 0.4018g of sodium metavanadate is disolved in 70mL of hot water and cooled to room temperature (very pale green solid ... makes a clear liquid)
  2. 1.6mL of 6M HCl is added (solution turns a beautiful golden color)
  3. 4.639g of Na12P2W15O56 is added slowly with vigorous stirring. (The solution tuned a deep red-orange color)
  4. Solution was stirred for 10 minutes
  5. 10.0369g of KCl was added to precipitate the POM
  6. Solid was removed by filtration. (I let the vacuum filtration go for an extra hour to try and dry the solid. But the solid was still quite wet when I collected it. Mass = 6.8293g)
  7. Solid was recrystallized from hot water (pH 1.5). (Started with around 15mL of water, removed from heat when crystals started appearing at around 7.5mL)
  8. Placed in the refrigerator over the weekend.

20130621 V+HCl.jpg Sodium metavanadate + HCl

20130621 V+HCl+W.jpg + Na12P2W15O56

20130621 V+HCl+W+KCl.jpg + KCl

20130621 V+HCl+W+KCl Recryst.jpg recrystallization of K8HP2W15V3O62-9H2O