User:Ellen Petersen/Notebook/MOF/2013/06/25

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==DPNI: 06-25-13==
==DPNI: 06-25-13==
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* 1.) Add solids 1,4,5,8 Naphthalenetetracarboxylic dianhydride (.805 g, 3.00 mmol) and 4-aminopyridine (.847 g, 6.00 mmol)to round bottom flask
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* 1.) Add solids 1,4,5,8 Naphthalenetetracarboxylic dianhydride (.805 g, 3.00 mmol) and 4-aminopyridine (.847 g, 6.00 mmol)to round bottom flask (I added .8051 g of 1,4,5,8 Naphthalenetetracarboxylic dianhydride, and .8481 g of 4-aminopyridine)
* 2.) Add 150 mL of solvent (DMA) ~keep under hood~
* 2.) Add 150 mL of solvent (DMA) ~keep under hood~
* 3.) Add Stir Bar to solution
* 3.) Add Stir Bar to solution
* 4.) Put under spout and raise black knob until there is enough pressure to hold it in place
* 4.) Put under spout and raise black knob until there is enough pressure to hold it in place
* 5.) Begin to stir
* 5.) Begin to stir
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* 6.) Vacuum out oxygen : turn big end of nossle up, observe that solution does react
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* 6.) If attached to condenser, turn on water very slightly
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* 7.) Turn off vacuum and turn on nitrogen: turn little end of nossle up. Bubbles in back should appear, this means nitrogen is on
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* 7.) Turn on nitrogen: ensure bubbles are about 1 every 4 seconds. (Turn little end of nossle up)
* 8.) Turn on heat to 56, switch down accordingly until it reaches 135 degrees consistently.  
* 8.) Turn on heat to 56, switch down accordingly until it reaches 135 degrees consistently.  
* 9.) If solution seems to be boiling adjust and turn down
* 9.) If solution seems to be boiling adjust and turn down
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*10.) Solution stable at 133 degrees at 51, mark red line on it to see difference in solution level.  
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* 10.) Solution stable at 134 degrees at 50, mark red line on it to see difference in solution level.  

Revision as of 10:09, 25 June 2013

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DPNI: 06-25-13

  • 1.) Add solids 1,4,5,8 Naphthalenetetracarboxylic dianhydride (.805 g, 3.00 mmol) and 4-aminopyridine (.847 g, 6.00 mmol)to round bottom flask (I added .8051 g of 1,4,5,8 Naphthalenetetracarboxylic dianhydride, and .8481 g of 4-aminopyridine)
  • 2.) Add 150 mL of solvent (DMA) ~keep under hood~
  • 3.) Add Stir Bar to solution
  • 4.) Put under spout and raise black knob until there is enough pressure to hold it in place
  • 5.) Begin to stir
  • 6.) If attached to condenser, turn on water very slightly
  • 7.) Turn on nitrogen: ensure bubbles are about 1 every 4 seconds. (Turn little end of nossle up)
  • 8.) Turn on heat to 56, switch down accordingly until it reaches 135 degrees consistently.
  • 9.) If solution seems to be boiling adjust and turn down
  • 10.) Solution stable at 134 degrees at 50, mark red line on it to see difference in solution level.



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