User:Ellen Petersen/Notebook/MOF/2013/06/26: Difference between revisions

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|style="background-color: #EEE"|[[Image:owwnotebook_icon.png|128px]]<span style="font-size:22px;"> Project name</span>
|style="background-color: #EEE"|[[Image:owwnotebook_icon.png|128px]]<span style="font-size:22px;"> MOF</span>
|style="background-color: #F2F2F2" align="center"|<html><img src="/images/9/94/Report.png" border="0" /></html> [[{{#sub:{{FULLPAGENAME}}|0|-11}}|Main project page]]<br />{{#if:{{#lnpreventry:{{FULLPAGENAME}}}}|<html><img src="/images/c/c3/Resultset_previous.png" border="0" /></html>[[{{#lnpreventry:{{FULLPAGENAME}}}}{{!}}Previous entry]]<html>&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;</html>}}{{#if:{{#lnnextentry:{{FULLPAGENAME}}}}|[[{{#lnnextentry:{{FULLPAGENAME}}}}{{!}}Next entry]]<html><img src="/images/5/5c/Resultset_next.png" border="0" /></html>}}
|style="background-color: #F2F2F2" align="center"|<html><img src="/images/9/94/Report.png" border="0" /></html> [[{{#sub:{{FULLPAGENAME}}|0|-11}}|Main project page]]<br />{{#if:{{#lnpreventry:{{FULLPAGENAME}}}}|<html><img src="/images/c/c3/Resultset_previous.png" border="0" /></html>[[{{#lnpreventry:{{FULLPAGENAME}}}}{{!}}Previous entry]]<html>&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;</html>}}{{#if:{{#lnnextentry:{{FULLPAGENAME}}}}|[[{{#lnnextentry:{{FULLPAGENAME}}}}{{!}}Next entry]]<html><img src="/images/5/5c/Resultset_next.png" border="0" /></html>}}
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==Entry title==
==DPNI: 06-26-13==
* Insert content here...
 
* 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 .8054 g of 1,4,5,8 Naphthalenetetracarboxylic dianhydride, and .8479 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 50, switch down accordingly until it reaches 135 degrees consistently.
* 9.) If solution seems to be boiling adjust and turn down
* 10.) Solution stable at 135 degrees at 35, mark red line on it to see difference in solution level.  
______________________________________________________________________________________________________
 
06-27-13
 
* 11.) Turn off nitrogen and water, Cool to Room Temperature
* 12.) Not enough diethyl ether, took 400 mL of diethyl ether (instead of the required 600 mL) and poured 2/3's of DPNI solution into the 400 mL of diethyl ether.
* 13.) Filter out
 
______________________________________________________________________________________________________
 
07-02-13
 
*14.) Ran 1/4 of the DPNI with 150 mL of ethanol through the rotavap
 
______________________________________________________________________________________________________
 
07-05-13
 
*15.) Ran the rest of the DPNI with 150 mL of ethanol through the rotavap
 




Revision as of 12:59, 8 July 2013

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DPNI: 06-26-13

  • 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 .8054 g of 1,4,5,8 Naphthalenetetracarboxylic dianhydride, and .8479 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 50, switch down accordingly until it reaches 135 degrees consistently.
  • 9.) If solution seems to be boiling adjust and turn down
  • 10.) Solution stable at 135 degrees at 35, mark red line on it to see difference in solution level.

______________________________________________________________________________________________________

06-27-13

  • 11.) Turn off nitrogen and water, Cool to Room Temperature
  • 12.) Not enough diethyl ether, took 400 mL of diethyl ether (instead of the required 600 mL) and poured 2/3's of DPNI solution into the 400 mL of diethyl ether.
  • 13.) Filter out

______________________________________________________________________________________________________

07-02-13

  • 14.) Ran 1/4 of the DPNI with 150 mL of ethanol through the rotavap

______________________________________________________________________________________________________

07-05-13

  • 15.) Ran the rest of the DPNI with 150 mL of ethanol through the rotavap



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