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.
- 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)
- 1.6mL of 6M HCl is added (solution turns a beautiful golden color)
- 4.639g of Na12P2W15O56 is added slowly with vigorous stirring. (The solution tuned a deep red-orange color)
- Solution was stirred for 10 minutes
- 10.0369g of KCl was added to precipitate the POM
- 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)
- 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)
- Placed in the refrigerator over the weekend.
Sodium metavanadate + HCl
recrystallization of K8HP2W15V3O62-9H2O