User:Matt Hartings/Notebook/Photosynthesis/2013/06/18

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POM synthesis

Performing the synthesis of Na12P2W18O56 from K6P2W18O62 and NaClO4 as described in Hartings_AU_Photosynthesis_Lab:Protocols/Na12P2W18O62 this protocol

Measured out 20.19g K6P2W18O62 (protocol calls for 20.00g)

Dissolved in 50 mL of water in beaker on stir plate (set to 80C) and cooled to room temperature.

15.409g NaClO4 added to the solution. A white ppt (KClO4) formed immediately.

This solution was allowed to stand for 1 hour. The ppt was filtered out and the green filtrate was retained.

1M Na2CO3 (21.1889g Na2CO3 in 200mL) was added dropwise until the pH reached 9.

The pH was maintained at 9 for an hour.

The product was filtered and the solid washed with 75mL of NaCl saturated water, 75mL of ethanol, and 75mL of diethyl ether.

The solid product was collected and placed in a dessicator (protocol calls for 2 days of dessication over H2SO4, I am drying it over dririte.)

Notes

  1. It took a bit of Na2CO3 addition before the solution kept a stable high pH
  2. The solution started losing its green color and a ppt formed as the pH started to reach a stable value of 8.1
  3. A pH of 9 was reached after roughly 60mL of 1M Na2CO3 added.
  4. A total of ~100 mL of 1M Na2CO3 was added through the whole process.


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