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 | ||
== | ==protocol== | ||
====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®ion=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®ion=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
protocolExchange of sodium montmorillonite for an organic cation 1-hexadecyl)triphenylphosphonium bromide
Preparation of XRD film
|
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.
- 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 tributylhexadecylphosphonium bromide or (1-hexadecyl)triphenylphosphonium bromide to exchange 100% of the Na from the clay.
- Add this amount of phosphonium ion to the clay solution.
- Cap the vial
- Stir for 1 week.
- Vacuum filter using 0.2uM nylon filter paper
- Dry in oven at 90C overnight
- Grind with a mortar and pestle.
- Store in a dessicator
|}