User:Michael S. Bible/Notebook/CHEM498 POMs/2015/11/19

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Objective

Adopting the protocol for the synthesis of [CeK(H2O)12][Ce(H2O)6]2[(H2O)4CeBW11O39H]2·20H2O, a synthesis was performed using Ce(NH4)4(SO4)4 ·2H2O rather than Ce(NO3)3.

Protocol

  • Dissolved 1.2883g (~2 mmol) Ce(NH4)4(SO4)4 ·2H2O in 20 mL of DI water.
  • Dissolved 1.6053g (~0.5 mmol) K8[BW11O39H]·13H2O in 40 mL of DI water.
  • Added the second solution to the first solution.
  • Verified pH was ~3.5
  • Refluxed solution with stirring for 2 hours at 80°C.
  • The resulting solution was saved for filtration on Thursday

Notes

  • When the solutions were mixed, they mixed without any precipitate (much like the reaction performed with Ceric Ammonium Nitrate).
  • Adjusting the pH prompted formation of local precipitate at site of NaOH addition.
  • Reflux solution was yellow and clear.
  • Solution was left overnight to be filtered on Monday.
  • During the time that the solution was left stirring until Monday, the solution became very cloudy (again, much like the reaction performed with Ceric Ammonium Nitrate).


Filtration of Ce(SO4)4 Reaction Mixture

  • The solution produced on 11/16 was also filtered and 0.4135g of precipitate was isolated.



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