User:Ellen Petersen/Notebook/MOF/2013/06/25: Difference between revisions
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==DPNI: 06-25-13== | ==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 | * 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 | ||
* 6.) | * 6.) If attached to condenser, turn on water very slightly | ||
* 7.) Turn | * 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 | ||
*10.) Solution stable at | * 10.) Solution stable at 134 degrees at 50, mark red line on it to see difference in solution level. | ||
Revision as of 08:09, 25 June 2013
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DPNI: 06-25-13
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