User:Karlena L. Brown/Notebook/PVOH Research/2013/04/03

PVOH Research

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OBJECTIVES Collect all DSC results from dry clay samples previously prepared on 2/08/13 Run DSC sample analysis on microsphere samples previously prepared on 3/29/13 Remove all excess oil from controlled microsphere samples prepared on 03/29/13 Run fluorescence analysis on all microsphere samples prepared 02/20/13 with Rhodamine 6G dye DSC Results for Dry Clay Samples DSC Analysis: Mixed Microspheres DSC preparation and protocol involving instrumentation and usage can be found on 9/17/12 entry. Sample Name Sample Mass (mg) Pan / Lid Mass (mg) 50:50 PVOH 130K NaMT 3.12 50.01 90:10 PVOH 130K 110% CEC NaMT w/ DMHXLBR 2.29 50.17 90:10 PVOH 130K Laponite 2.59 50.12 90:10 PVOH 130K 110% CEC Laponite w/ DMHXLBR 2.27 50.28 90:10 PVOH 146K 110% CEC NaMT w/ DMHXLBR 2.65 50.11 50:50 PVOH 146K 110% CEC NaMT w/ DMHXLBR 2.50 50.17 Specific DSC parameters and protocols set to analyze dry clay samples included the following: # Equilibrate sample at ~ -40°C # Ramp sample temperature up from 20-240°C # Ramp sample temperature down from 20-(-40°C) # Repeat segment #2 again Fluorescence Analysis: Diffusion Testing 2 RECALL DIFFUSION TESTING PROTOCOL ON 2/15/13 Fluorescent samples run and completed for 2hr diffusion rate determinations: # Microsphere 90:10 PVOH 146K 50% CEC NaMT w/ Bu3HdP+ # Microsphere 90:10 PVOH 146K 110% CEC Laponite w/ DMHXLBR # Microsphere 90:10 PVOH 146K NaMT # Microsphere 50:50 PVOH 146K NaMT # Microsphere 50:50 PVOH 146K 50% CEC NaMT w/ Bu3HdP+ # Microsphere 50:50 PVOH 146K 110% CEC Laponite w/ DMHXLBR Specific parameters used to analyze fluorescence of hydrogel samples containing Rhodamine 6G dye included the following: # Excitation: 480nm # Emission Range: 500-650nm # Excitation Slit Width: 10 # Emission Slit Width: 10 # Scan Speed: 1200 Fluorescence Results & Spectrums Figure 1 - Microsphere 90:10 PVOH 146K 50% CEC NaMT w/ Bu3HdP+ ***Fluorescence intensity maximum is 6.985 Figure 2 - Microsphere 90:10 PVOH 146K 110% CEC Laponite w/ DMHXLBR ***Fluorescence intensity maximum is 5.109 Figure 3 - Microsphere 90:10 PVOH 146K NaMT ***Fluorescence intensity maximum is 26.734 Figure 4 - Microsphere 50:50 PVOH 146K NaMT ***Fluorescence intensity maximum is 17. Figure 5 - Microsphere 50:50 PVOH 146K 50% CEC NaMT w/ Bu3HdP+ ***Fluorescence intensity maximum is 11.661 Figure 6 - Microsphere 50:50 PVOH 146K 110% CEC Laponite w/ DMHXLBR ***Fluorescence intensity maximum is 137.319 Notes For many of the DSC samples run, the microsphere samples analyzed were not completely dry; therefore, the DSC peak analysis will be highly affected by the presence of safflower oil encompassed in the sample X-ray diffraction will be run on all prepared microsphere samples in order to determine whether clay has agglomerated separately from the PVOH For hydrophilic polymers blended with clay, it was referenced that a peak shift below 10° was a strong indicator of excellent conglomeration The microsphere prepared with 50:50 PVOH 146K 110% CEC Laponite w/ DMHXLBR caused the most diffusion of dye All microspheres will be used for pressure testing, however, because not all dye leaked out