User:Karlena L. Brown/Notebook/PVOH Research/2012/10/31

PVOH Research

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OBJECTIVES Frepare PVOH film with 5-hydroxymethylfurfural Run FTIR analysis on all films prepared throughout the semester Run ion diffusion experiment on PVOH film and analyze data using Ion Selective Electrode Furfural Film Preparation In 10mL beaker, weigh out ~ 1.0 grams PVOH (MW 22K) (PVOH 22K Actual Mass = 1.0029g) Then, using a graduated cylinder add ~ 5 mL H2O to the beaker After adding and combining PVOH (MW 22K) in a small beaker with H2O, add a stir bar and prepare to stir solution On hot plate, stir and heat beaker solutions at 70-80°C for ~ 12 min or until PVOH dissolves Once PVOH solids thoroughly dissolve in solution, take the solution and place it in the fume hood Allow the solution to cool then add ~ 0.3g of 5-hydroxymethylfurfural to the solution (Furfural Actual Mass = 0.3192g) Then pour the solution into a Teflon dish to sit, cool, and dry in the fume hood for ~ 2 days Films Examined using FTIR RECALL FTIR PROCEDURAL PROTOCOL 9/17/12 LIST OF FILMS FOR FTIR: Films New mass(g) PVOH(22K) 1.0067g+1mL GA+1mL porphyrin crosslinked 1.7688 PVOH(22K)+0.5mL GA+0.104g NaMT crosslinked spun 10 min CuSO4 prepared 10/17/2012 0.9465 PVOH(22K)+0.5mLGA+0.99mL porphyrin(no color on film )crosslinked prepared 10/19/2012 1.8045 PVOH(22K)+1mL GA+100%CEC crosslinked prepared 10/4/2012 1.3662 PVOH(22K)+1mL GA+1mL porphyrin crosslinked prepared 10/24/2012 1.5477 PVOH(22K)+0.5mL GA+1mL porphyrin crosslinked prepared 10/24/2012 #2 1.9685 PVOH(22K)+0.5mLGA+1mL porphyrin prepared crosslinked 10/26/2012 2.1206 PVOH(22K)+0.8wt% GA+100%CEC crosslinked spun 10 min CuSO4 prepared 10/26/2012 1.24 PVOH(22K)+0.8wt% GA+50% CEC crosslinked spun 10 min CuSO4 prepared 10/17/2012 1.074 Ion Diffusion & Ion Selective Electrode Film Procedures Cut small piece of PVOH 22K film containing 1mL glutaldehyde exchanged in CuSO4 for 10 min Place small cut piece of PVOH 22K film in plastic double graduated cylinder apparatus Close and seal plastic double graduated cylinder apparatus Next, in one graduated cylinder column pour in ~ 20mL of HPLC Grade H2O Then, in other graduated cylinder column pour in ~20mL of the varied ion concentrated solution Plug the electrodes into the SympHony meter and turn on the ion selective electrode instruments Then press the arrows until ISE (ion selective electrode) and μS/cm (microsiemen per centimeter) appear on the screen Remove the electrodes from the storage solutions Rinse the electrodes with distilled H2O and thoroughly dry both with KimWipes Place each electrode directly into the graduated cylinder columns containing either the HPLC Grade H2O or the varied ion solution for analysis (one electrode per graduated column) Measure the total amount of solution available and present for each graduated cylinder column Let each solution and electrode equilibrate for a set period of time (between 2-5 minutes) and then press measure on each instrument Once the measurement is finalized, record the values observed for each solution Ensure the hole separating the two graduated cylinder columns is completely shielded and covered by the PVOH 22K film Ion Diffusion Film Analysis: Varied Ion Solution A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO4 solution was used for an Ion Selective Electrode Analysis. Time Recordings Initial Volume(mL) Final Volume (mL) Conductivity (μS/cm) 8:50A 30 30 864 9:00A 30 30 869 9:30A 30 30 874 10:00A 30 30 865 10:30A 30 30 863 11:00A 30 29.5 861 11:30A 29.5 30 858 12:00P 30 30 853 3:15P 30 29.8 840 9:00P 29.8 28 819 Ion Diffusion Film Analysis: HPLC Grade H2O Solution A crosslinked PVOH 22K film containing 1mL glutaldehyde that had been exchanged for 10 min in the CuSO4 solution was used for an Ion Selective Electrode Analysis. Time Recordings Initial Volume(mL) Final Volume (mL) Conductivity (μS/cm) 8:50A 28 28 19.93 9:00A 28 29 23.13 9:30A 29 29 24.60 10:00A 29 28.5 27.20 10:30A 28.5 29 30.5 11:00A 29 29 33 11:30A 29 29 35.7 12:00P 29 29 38.9 3:15P 29 28.6 52.7 9:00P 28.6 27.2 76.2 Notes The varied ion concentrated solution contained the following ions: Chlorine (Cl-), Bromine (Br-), and Iodine (I-). μS/cm (microsiemen per centimeter) is a conductivity unit of measurement that is the inverse of an Ohm (O). Experimental readings regarding the Ion Selective Electrode Analysis were taken every 30 minutes; however, for the first reading and recording only a 10 min interval surpassed before a reading was taken. The final two readings germane to the Ion Selective Electrode Analysis for the PVOH 22K film containing 1mL glutaldehyde that was exchanged for 10 min with CuSO4 were taken by Dr. Fox. A small leak was detected in the film used after several hours had passed (9:00P).