User:Moira M. Esson/Notebook/CHEM-581/2012/11/02: Difference between revisions

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FTIR Film preparation:
FTIR Film preparation:
General protocol for the preparation of crosslinked glutaraldehyde films for FTIR:
*Crosslinked glutaraldehyde films were patted dry with a paper towel, had a small portion cut off and placed in a 10mL beaker to completely dry. The remaining large portion of the film was reweighed and placed in a beaker filled with deionized H<sub>2</sub>O for further storage.
*Crosslinked glutaraldehyde films were patted dry with a paper towel, had a small portion cut off and placed in a 10mL beaker to completely dry. The remaining large portion of the film was reweighed and placed in a beaker filled with deionized H<sub>2</sub>O for further storage.
Prepared films:
Prepared films:

Revision as of 19:22, 10 November 2012

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Objectives

  1. Prepare new solutions for UV-Vis
  2. Soak prepared furfural film in ethyl acetate
  3. Run prepared solutions on UV-Vis(run baseline with HPLC grade H2O
  4. Rerun ion selective electrodes


Furfural Films

General Protocol for rinsing of furfural films:

  1. Place magnetic stir bar and stemless Büchner funnel top into a 150mL beaker
  2. Remove film from Teflon dish and place into the beaker
  3. Add at least 100mL reagent grade ethyl acetate to the beaker(need enough ethyl acetate to completely cover the film)
  4. Allow the ethyl acetate solution to stir until it appears no color is leaking out from the film


  • The furfural film prepared on 10/31/2012 followed the general protocol for rinsing of fufural films.
  • The fufural film was spin in EtAc for 2.5hours

Observations:

  • Before placement in the ethyl acetate, the film was a dark brown color(uniformly distributed throughout the film) and was very rigid. So rigid slight cracking appeared to be occurring toward the edge of the film
  • While in the ethyl acetate, approximately 2 hours into the stirring, slight leakage of furfural from the film. Very slight(perhaps no leakage at all). Some of the ethyl acetate solution was placed in a falcon tube for later analysis.
  • After 2.5hrs in the ethyl acetate, film was still dark brown colored and extremely rigid


FTIR

  • The general protocol for FTIR was followed

Ran films:

  1. PVOH(22K)+1mL GA+100% CEC(prepared 10/3/2012)
  2. PVOH(22K)+1mL GA+50% CEC(prepared 10/4/2012)
  3. PVOH(22K)+1mL GA+NaMT(prepared 10/3/2012)
  4. dehydrated crosslinked PVOH(22K)+1mL GA spun 10 min in CuSO4 (prepared 10/13/2012)
  5. Thin FTIR film(0.1000g PVOH 22K)(prepared 9/21/2012)
  6. PVOH(22K)+1mL GA (prepared 10/3/2012)
  7. PVOH(22K)+0.3199 furfural+HCl(after spun with ethyl acetate)

FTIR Images from previous runs:

FTIR Film preparation: General protocol for the preparation of crosslinked glutaraldehyde films for FTIR:

  • Crosslinked glutaraldehyde films were patted dry with a paper towel, had a small portion cut off and placed in a 10mL beaker to completely dry. The remaining large portion of the film was reweighed and placed in a beaker filled with deionized H2O for further storage.

Prepared films:

Films New mass(g)
PVOH(22K)+0.5mL GA+100% CEC crosslinked prepared 10/19/2012 3.1554
PVOH(22K)+0.8wt% GA+100%CEC crosslinked prepared 10/3/2012 0.3478
PVOH(22K)+1mL GA+50% CEC crosslinked prepared 10/4/2012 0.9595
PVOH(22K)+0.5mL GA+NaMT crosslinked prepared 10/19/2012 2.4191

UV-vis

  • Ran UV-vis on all prepared porphyrin solutions(including solutions with various salt additives) and solutions from crosslinking

Sodium Ion selective electrode

  • The general protocol for ion selective electrodes was followed
  • The film which was used on 10/31/2012 for ion selective electrode was stored in deionized H2O was tested

Results:

Amount of H2O film stored in(mL) 49.8
ISE values(mV) -96.1
Conductivity(μS/cm) 70.2


Notes:

  • Appears that there is a higher concentration than from 15ppm Cu2+ measured on 2012/10/03


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