User:Eleni N. Kalivas/Notebook/CHEM-571/2014/09/10: Difference between revisions

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*Start exchange of sodium montmorillonite for an organic cation
*Start exchange of sodium montmorillonite for an organic cation


==Description==
==protocol==
We are going to exchange the sodium in the sodium montmorillonite for an organic cation. The procedures are taken from these two sources ([http://www.scirp.org/journal/PaperInformation.aspx?PaperID=17245#.VA5V9Et5_zY 1], [http://www.clays.org/journal/archive/volume%2010/10-1-153.pdf 2] along with Karlena Brown's thesis. We are working from the starting point that there are 92 miliequivalents (meq) of Na+ per 100g of montmorillonite.


====Exchange of sodium montmorillonite for an organic cation 1-hexadecyl)triphenylphosphonium bromide====
# Add 1.1014g of Sodium Montmorillonite (NaMT) to a scintillation vial containing 20mL of 50:50 HPLC grade water:ethanol.  
# Add 1.1014g of Sodium Montmorillonite (NaMT) to a scintillation vial containing 20mL of 50:50 HPLC grade water:ethanol.  
# Determine the amount of cation to add if using either [http://www.sigmaaldrich.com/catalog/product/aldrich/276200?lang=en&region=US tributylhexadecylphosphonium bromide] or [https://us.vwr.com/store/catalog/product.jsp?product_id=7491057 (1-hexadecyl)triphenylphosphonium bromide] to exchange 100% of the Na from the clay.
# Determine the amount of cation to add if using either [http://www.sigmaaldrich.com/catalog/product/aldrich/276200?lang=en&region=US tributylhexadecylphosphonium bromide] or [https://us.vwr.com/store/catalog/product.jsp?product_id=7491057 (1-hexadecyl)triphenylphosphonium bromide] to exchange 100% of the Na from the clay.
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# Store in a dessicator
# Store in a dessicator


====Preparation of XRD film====
#Powder XRD will be taken of the plane NaMT
#XRD of a plane PVA film will also be taken
#XRD of a film soaked in 2ppm, 8ppm, 80ppm, and 200ppm will also be taken
##200ppm, this film was prepared by [[User:Michael S. Bible/Notebook/581/2014/09/10|Michael Bible's]] Notebook
##80ppm, A PVA-film was soaked in 10mL of 80ppm and left to soak until XRD analysis
##8ppm, This film was prepared by [[User:Madeleine Y. Bee/Notebook/CHEM-581 Experimental Chemistry/2014/09/10|Madeline Bee's]] Notebook
##2ppm, this film was prepared by [[User:James C. Schwabacher/Notebook/CHEM-571/2014/09/10|James Schwabacher's]] Notebook
*This data will allow us to discover which layer of the film the dye is being absorbed first, as eel as any changes in the clay structure.


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Revision as of 12:10, 12 September 2014

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Objective

  • Finish film synthesis
  • Start exchange of sodium montmorillonite for an organic cation

protocol

Exchange of sodium montmorillonite for an organic cation 1-hexadecyl)triphenylphosphonium bromide

  1. Add 1.1014g of Sodium Montmorillonite (NaMT) to a scintillation vial containing 20mL of 50:50 HPLC grade water:ethanol.
  2. Determine the amount of cation to add if using either tributylhexadecylphosphonium bromide or (1-hexadecyl)triphenylphosphonium bromide to exchange 100% of the Na from the clay.
  3. Add this amount of phosphonium ion to the clay solution.
  4. Cap the vial
  5. Stir for 1 week.
  6. Vacuum filter using 0.2uM nylon filter paper
  7. Dry in oven at 90C overnight
  8. Grind with a mortar and pestle.
  9. Store in a dessicator

Preparation of XRD film

  1. Powder XRD will be taken of the plane NaMT
  2. XRD of a plane PVA film will also be taken
  3. XRD of a film soaked in 2ppm, 8ppm, 80ppm, and 200ppm will also be taken
    1. 200ppm, this film was prepared by Michael Bible's Notebook
    2. 80ppm, A PVA-film was soaked in 10mL of 80ppm and left to soak until XRD analysis
    3. 8ppm, This film was prepared by Madeline Bee's Notebook
    4. 2ppm, this film was prepared by James Schwabacher's Notebook


  • This data will allow us to discover which layer of the film the dye is being absorbed first, as eel as any changes in the clay structure.


Description

We are going to exchange the sodium in the sodium montmorillonite for an organic cation. The procedures are taken from these two sources (1, 2 along with Karlena Brown's thesis. We are working from the starting point that there are 92 miliequivalents (meq) of Na+ per 100g of montmorillonite.

  1. Add 1.1014g of Sodium Montmorillonite (NaMT) to a scintillation vial containing 20mL of 50:50 HPLC grade water:ethanol.
  2. Determine the amount of cation to add if using either tributylhexadecylphosphonium bromide or (1-hexadecyl)triphenylphosphonium bromide to exchange 100% of the Na from the clay.
  3. Add this amount of phosphonium ion to the clay solution.
  4. Cap the vial
  5. Stir for 1 week.
  6. Vacuum filter using 0.2uM nylon filter paper
  7. Dry in oven at 90C overnight
  8. Grind with a mortar and pestle.
  9. Store in a dessicator


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