User:Paul Rothenberg/Notebook/Pauls Notebook/2013/05/28: Difference between revisions

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==28 May 2013==
==Reaction of OPD and H2O2 in Water with Mb/Citrate Catalyst==
* Objectives
* Objectives
*1. Continue analysis of OPD+H2O2 with Mb Citrate with H<sub>2</sub>O as a solvent
*1. Continue analysis of OPD+H2O2 with Mb Citrate with H<sub>2</sub>O as a solvent
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*Procedure:
*Procedure:


*1. Same protocol as [5/20-5/24] using H<sub>2</sub>O instead of MeOH
*1. Same protocol as [http://openwetware.org/wiki/User:Paul_Rothenberg/Notebook/Pauls_Notebook/2013/05/20#20_May_2013 5/20] using H<sub>2</sub>O instead of MeOH




*Data:
*Data:


[[Image:Mb_Citrate_H2O_5C_WORKUP_GRAPH.png]]
[[Image:Mb_Citrate_H2O_5C_WORKUP_GRAPH.png|375px]] [[Image:Mb_Citrate_H2O_5C_Sequential_WORKUP_GRAPH.png|375px]] <br>


[[Image:Mb_Citrate_H2O_5C_Sequential_WORKUP_GRAPH.png]]
[[Image:Mb_Citrate_H2O_15C_WORKUP_GRAPH.png|375px]] [[Image:Mb_Citrate_H2O_15C_Sequential_WORKUP_GRAPH.png|375px]] <br>


[[Image:Mb_Citrate_H2O_15C_WORKUP_GRAPH.png]]
[[Image:Mb_Citrate_H2O_25C_WORKUP_GRAPH.png|375px]] [[Image:Mb_Citrate_H2O_25C_Sequential_WORKUP_GRAPH.png|375px]] <br>


[[Image:Mb_Citrate_H2O_15C_Sequential_WORKUP_GRAPH.png]]
[[Image:Mb_Citrate_H2O_35C_WORKUP_GRAPH.png|375px]] [[Image:Mb_Citrate_H2O_35C_Sequential_WORKUP_GRAPH.png|375px]] <br>


[[Image:Mb_Citrate_H2O_25C_WORKUP_GRAPH.png]]
[[Image:Mb_Citrate_H2O_45C_WORKUP_GRAPH.png|375px]] [[Image:Mb_Citrate_H2O_45C_Sequential_WORKUP_GRAPH.png|375px]] <br>


[[Image:Mb_Citrate_H2O_25C_Sequential_WORKUP_GRAPH.png]]
==Synthesis of Na<sub>12</sub>P<sub>2</sub>W<sub>18</sub>O<sub>62</sub>==


[[Image:Mb_Citrate_H2O_35C_WORKUP_GRAPH.png]]


[[Image:Mb_Citrate_H2O_35C_Sequential_WORKUP_GRAPH.png]]
Synthesis of Na<sub>12</sub>P<sub>2</sub>W<sub>18</sub>O<sub>62</sub> is crucial for synthesizing polyoxometalates.<sup>1</sup> We will be synthesizing POMs in the following weeks, and the preparatory reactions will be set up soon. The protocol for this reaction can be found [http://openwetware.org/wiki/Hartings_AU_Photosynthesis_Lab:Protocols/K6P2W18O62 here].  
 
[[Image:Mb_Citrate_H2O_45C_WORKUP_GRAPH.png]]
 
[[Image:Mb_Citrate_H2O_45C_Sequential_WORKUP_GRAPH.png]]
 
 
 
 
 
 
 
*Synthesis of Na<sub>12</sub>P<sub>2</sub>W<sub>18</sub>O<sub>62</sub>:
 
 
*Synthesis of Na<sub>12</sub>P<sub>2</sub>W<sub>18</sub>O<sub>62</sub> is crucial for synthesizing polyoxometalates.<sup>1</sup> We will be synthesizing POMs in the following weeks, and the preparatory reactions will be set up soon.




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*1. 100 grams of Na<sub>2</sub>WO<sub>4</sub>*2H<sub>2</sub>O was added to 350 mL of water and boiled
*1. 100 grams of Na<sub>2</sub>WO<sub>4</sub>*2H<sub>2</sub>O was added to 350 mL of water and boiled
*2. 150 mL of 85% H<sub>3</sub>PO<sub>4</sub> was slowly added dropwise to the solution
*2. 150 mL of 85% H<sub>3</sub>PO<sub>4</sub> was slowly added dropwise to the solution
<sub>Began dropping H<sub>3</sub>PO<sub>4</sub> at 3:30, dropped for approximately 20 minutes</sub>
<sub>Began dropping H<sub>3</sub>PO<sub>4</sub> at 3:30, dropped for approximately 15 minutes</sub>
*3. The resulting yellow-green solution was refluxed overnight (5-13 hours indicated<sup>1</sup>).  
*3. The resulting yellow-green solution was refluxed overnight (5-13 hours indicated<sup>1</sup>).  



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Reaction of OPD and H2O2 in Water with Mb/Citrate Catalyst

  • Objectives
  • 1. Continue analysis of OPD+H2O2 with Mb Citrate with H2O as a solvent
  • Procedure:
  • 1. Same protocol as 5/20 using H2O instead of MeOH


  • Data:






Synthesis of Na12P2W18O62

Synthesis of Na12P2W18O62 is crucial for synthesizing polyoxometalates.1 We will be synthesizing POMs in the following weeks, and the preparatory reactions will be set up soon. The protocol for this reaction can be found here.


  • Procedure:
  • 1. 100 grams of Na2WO4*2H2O was added to 350 mL of water and boiled
  • 2. 150 mL of 85% H3PO4 was slowly added dropwise to the solution

Began dropping H3PO4 at 3:30, dropped for approximately 15 minutes

  • 3. The resulting yellow-green solution was refluxed overnight (5-13 hours indicated1).


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