User:Klare Lazor/Notebook/Chem-496-001/2013/02/04: Difference between revisions

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#synthesize quaternary ammonium
#synthesize quaternary ammonium


==Description==
==Description and Data==
'''Cross-linking PVOH+Isopropyl+glutaraldehdye'''
'''Cross-linking PVOH+Isopropyl+glutaraldehdye'''


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'''Synthesis of Ammonium Salt'''
'''Synthesis of Ammonium Salt a 2 fold reaction'''
*Added 4-chloro-1-butanol (Eastman) and Triethylamine in acetonitrile for 3 days to reflux.   
*Added 4-chloro-1-butanol (Eastman) and Triethylamine in acetonitrile for 72 hours to reflux.   
<b>[[User:Matt Hartings|Matt Hartings]] I need more than this, Klare. How much did you add? The reaction is stirring. It's running under nitrogen. You're heating with a heating mantle. This is the first time you've done this, and, certainly, the first time its shown up in your lab notebook. I need a little bit more than this.</b>
* SN2 reaction
*Added 10mL of Acetonitrile and 1.148mL chlorobutanol and 0.753ml triethylamine in round bottom flask with stir bar
*Attached flask to a redox condense.
* heated with a heating mantle with sand
*set 100v heater to 50 because of evap temp for acetonitrile should occur around that voltage
*Added nitrogen gas to flow through reflux condenser such that the run occurs under nitrogen.  
*turned on heating mantle and left the flask to reflux for 72 hours


'''Results of films after cross linking'''
'''Image of SN2 reaction'''
*No sodium sulfate high molecular weight low solubility.... Don't use both can use either... DSC and IR still
*Isopropyl evaporate off before it could cross link over the weekend
*phenol or benzyl alcohol soluble in water
*1 gram 
*Were tearing need DSC and IR. Prediction of isopropyl evaporate from the films over the weeked :(


==Data==
[[Image:Screen_Shot_2013-02-06_at_12.56.03_AM.png]]
* Add data and results here...


==Notes==
This area is for any observations or conclusions that you would like to note.


'''Results of films after cross linking'''
*Isopropyl evaporate off before we could cross link the film after the weekend. Could tell because films were very water soluble and were falling apart in sodium bicarbonate solution.  Except for the glutaraldehyde control.
*phenol or benzyl alcohol soluble in water can be used because will remain in film long enough to cross-link
*Next time films will contain 1 gram of pvoh because prior films were way to thin.


Use categories like tags. Change the "Course" category to the one corresponding to your course. The "Miscellaneous" tag can be used for particular experiments, as instructed by your professor. Please be sure to change or delete this tag as required so that the categories remain well organized.


[[Category:Course]]
[[Category:Miscellaneous]]




[[Category:Course]]
[[Category:Miscellaneous]]


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Revision as of 23:02, 5 February 2013

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Objective

  1. Cross‐link films
  2. Make more fixant
  3. DSC and FTIR after cross-­‐linking.
  4. synthesize quaternary ammonium

Description and Data

Cross-linking PVOH+Isopropyl+glutaraldehdye

  1. Allow the PVOH film containing glutaraldehyde to dry completely.
  2. Prepare a solution of 100 mL H2O, 2 mL concentrated H2SO4, and 20 g Na2SO4 in a 150 mL beaker. (solution is referred to as glutaraldehyde fixant)
  3. Place stir bar in beaker and a Buchner funnel top (cap) over the stir bar
  4. Heat solution to 70°C (temperature on hotplate should be about 160)
  5. Place film in solution for one hour.
  6. Prepare 100 mL of a 1% HCl solution in a 150 mL beaker. Place a stir bar and an inverted buchner funnel into beaker.
  7. Heat HCl solution to 70°C
  8. Remove film from glutaraldehyde fixant and rinse with distilled water.
  9. Place film into HCl solution for 30 minutes.
  10. Prepare 0.2 M sodium bicarbonate solution. (1.68 g in 100 mL)
  11. After 30 minutes, remove the film from the HCl solution and place into the sodium bicarbonate solution (at room temperature) for about 15 minutes.
  12. Use tweezers to remove the film from the sodium bicarbonate solution.
  13. Rinse film with deionized water and place in a beaker with distilled water until it is used/tested


Synthesis of Ammonium Salt a 2 fold reaction

  • Added 4-chloro-1-butanol (Eastman) and Triethylamine in acetonitrile for 72 hours to reflux.
  • SN2 reaction
  • Added 10mL of Acetonitrile and 1.148mL chlorobutanol and 0.753ml triethylamine in round bottom flask with stir bar
  • Attached flask to a redox condense.
  • heated with a heating mantle with sand
  • set 100v heater to 50 because of evap temp for acetonitrile should occur around that voltage
  • Added nitrogen gas to flow through reflux condenser such that the run occurs under nitrogen.
  • turned on heating mantle and left the flask to reflux for 72 hours

Image of SN2 reaction


Results of films after cross linking

  • Isopropyl evaporate off before we could cross link the film after the weekend. Could tell because films were very water soluble and were falling apart in sodium bicarbonate solution. Except for the glutaraldehyde control.
  • phenol or benzyl alcohol soluble in water can be used because will remain in film long enough to cross-link
  • Next time films will contain 1 gram of pvoh because prior films were way to thin.




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