User:Moira M. Esson/Notebook/CHEM-581/2012/10/17

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Objectives

  1. Finish AA
  2. UV-Vis Cu2+ absorption solutions(blue stock solution that had prepared and filtrates). Using this to determine the detection limits of different instruments
  3. Cu2+ absorption using approximately 1g film(PVOH MW 22,000, PVOH MW 22,000+NaMT, PVOH+CEC)
  4. UV-Vis calibration curve for porphyrin soluitons(max absorbance should be 1)
  5. Make porphyrin films

Film Preparation

  • The general protocol for film preparation was followed. Films in which porphyrin was added, the general protocol for glutaraldehyde films was followed. Porphyrin was added after the addition of glutaraldehyde(GA). The reaction mixture was allowed to spin for ~1min. in order to create and equal distribution of porphyrin.

Films Prepared:

  1. PVOH(MW 22K)+GA 0.5mL+porphyrin 1mL
  2. PVOH(MW 22K)+GA 0.5mL+ 1.0124g NaMT
  3. PVOH(MW 22K)+GA 0.5mL+ 1.0007g 50%CEC
  4. PVOH(MW 22K)+GA 0.5mL+ 1.0006g 100%CEC

Observations:

  • The addition of porphyrin caused the film to become a light red/ pinkish color


UV-Vis of Porphyrin

Preparation of Porphyrin solution

  • All solutions were prepared by Melissa Novy. Please refer to Melissa Novy's notebook for explicit calculations
  1. 9 mL of water was added to 1mL of 94.45μM solution. The water and solution was placed in a tinted tube
  2. Using a series of 10 fold serial dilutions, 10mL solutions of 9.445 nM, 94.45nM and 944.5nM porphyrine solutions were prepared
  3. Absorption spectra of 9.445 nM, 94.45nM and 944.5nM porphyrine solutions were taken using a Shimadzu 2550 spectrophotometer.
  • A slit width of 1.0 nm
  • A glass/quartz cuvette was used
  • Baseline was conducted with a blank/empty cuvette


Image:Porphine_Absorbance.png

  • 9.445nM seems to be too dilute. It did not produce peaks. It appears that 944.5 nM porphine will produce the most useful data

Cu2+ adsorption

The general protocol for filtrates described on 2012/09/26. Instead of using prepared clays, however ~1g of prepared film was placed in the CuSO4 solution. Filtrate was only collected in 10min intervals

Type of film used mass of film used(g) weight of film after 10min (g)
PVOH(MW 22,000)+ 100% CEC1.481.0041
PVOH(MW 22,000)0.90.7582
PVOH(MW 22,000)+NaMT0.99450.9115
PVOH(MW 22,000)+ 50% CEC1.11671.0464

Notes

Unable to run AA. Solutions need to be reprepared next time and AA needs to be rerun.


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