User:Karlena L. Brown/Notebook/PVOH Research/2012/10/17

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OBJECTIVES

  • Make PVOH films with NaMT, 50% CEC NaMT, & 100% CEC NaMT for Cu2+ film adsorption
  • Measure UV-Vis of all porphyrin solutions (9.445nM – 9.445μM)
  • Make PVOH films containing tetra (4-sulfonatophenyl) porphine dihydrogen chloride (PORPHYRIN)

Preparations For Cu2+ Film Exchanged Solutions & Vacuum Filtration Procedures

RECALL PROCEDURAL PROTOCOL FOR Cu2+ FILM EXCHANGED SOLUTIONS & VACUUM FILTRATION PROCEDURES 10/05/12; however, instead of using clay, use ~ 1g films prepared containing PVOH, glutaldehyde, and clay samples. In addition, only exchange films for solely 10min time interval.

Films Prepared Original Film Mass (g) Film Mass After 10 min Exchange (g)
PVOH 22K 0.9000 0.7582
PVOH 22K w/ NaMT 0.9945 0.9115
PVOH 22K w/ 50% CEC NaMT 1.1167 1.0464
PVOH 22K w/ 100% CEC NaMT 1.1480 1.0041

UV - Vis Procedures

  1. Open UV-Vis Pro program on the computer
  2. Hit the UV-Vis switch at the bottom of the computer setup
  3. On the bottom of computer screen, click connect button
  4. Go through UV-Vis Safety Connection Procedures and Protocols for ~ 15 min
  5. Once finished safety protocol run, click method button
  6. Select a instrument scanning range (wavelengths = 200 - 800nm)
  7. Click data window button to create new folder → CHEM 581 → MKM
  8. Create name for sample run under new folder MKM
  9. Prepare a baseline (blank) sample to run in UV-Vis
  10. Use quartz cuvette specially made for UV-Vis and fill cuvette ¾ full with HPLC grade H2O
  11. Wipe quartz cuvette gently and thoroughly with a Kim Wipe
  12. Place cuvette in reference pocket of six sample UV-Vis instrument
  13. Approve selection and file name then click baseline button
  14. Run baseline of blank sample (HPLC grade H2O)
  15. Once finished running, autoscale the y-axis on the screen until max absorption = 1.0
  16. Save sample name under new folder MKM


Repeat procedure for all UV-Vis Samples run; however, do not have to run a baseline every time after each sample. Baseline only has to be run once throughout the total analysis. Also please be sure to clean each cuvette and wipe thoroughly each time before running new samples for analysis. In addition, place actual samples that are not references in the first pocket of six sample holder in UV-Vis.

Porphyrin Dilution Calculations

STOCK SOLUTION PORPHYRIN STARTED WITH CONCENTRATION OF 94.45μM, DILUTE SOLUTION TO GIVEN CONCENTRATIONS LISTED

  • Solution of 9.445 μM porphyrin
   (94.45 μM)(V1)=(9.445 μM)(10mL)
    V1 = 1mL of 94.45 μM porphyrin
  • Solution of 944.5 nM porphyrin
   (9.445 μM)(V1)=(944.5 nM)(10mL)
    V1 = 1mL of 9.445 μM porphyrin
  • Solution of 94.45 nM porphyrin
   (944.5 nM)(V1)=(94.45 nM)(10mL)
    V1 = 1mL of 944.5 nM porphyrin
  • Solution of 9.445 nM porphyrin
   (944.5 nM)(V1)=(9.445 nM)(10mL)
    V1 = 0.1mL of 944.5 nM porphyrin
  • Solution of 1.89 μM porphyrin
   (94.45 μM)(V1)=(1.89 μM)(10mL)
    V1 = 0.2mL of 94.45 μM porphyrin
  • Solution of 3.78 uM porphyrin
   (94.45 μM)(V1)=(3.78 μM)(10mL)
    V1 = 0.4mL of 94.45 μM porphyrin

UV-Vis of Porphyrin Solutions

  • Using a Shimadzu UV-2550 spectrophotometer, spectra of four concentrations of porphyrin solutions were taken:
 * Wavelength range = 200 - 800nm
 * Slit width = 1.0nm

UV-Vis Analysis Notes

  • The baseline was conducted with nothing in the cell.
  • For solutions at concentrations 944.5nM and 94.45nM, two peaks were visible at 410nm and 430nm.
  • The 9.445nM was not concentrated enough to produce any peaks.
  • The 944.5nM solution displayed several more peaks past 500nm, producing more useful data.
  • The concentrations of 31.48μM and 62.97μM proved to be too high in concentration; absorbency values were greater than 1.0 for each solution.

Porphyrin Film Preparations

Follow procedural protocol for preparing glutaldehyde films 9/19/12; however, add ~ 1mL of porphyrin in addition to glutaldehyde to each film before pouring substance into a Teflon dish. Also for two PVOH films, be sure to add two drops of HCl to observe if the addition of the acid aids in securing all of the porphyrin within the films.

Films Prepared PVOH 22K Amount (g) Glutaldehyde Amount (mL) Porphyrin Amount (mL) HCl Addition (Y/N)
PVOH 22K w/ GA & PP(g) 1.0073 1.0 1.0 N
PVOH 22K w/ GA & PP(g) 1.0067 1.0 1.0 Y
PVOH 22K w/ GA & PP(g) 1.0523 0.5 1.0 N
PVOH 22K w/ GA & PP(g) 1.0211 0.5 1.0 Y


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