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

PVOH Research

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