User:Eleni N. Kalivas/Notebook/CHEM-571/2015/02/13

PVA-Alg Bead Synthesis

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February 13, 2015 Upscale syntheses of PVA-Alg-NaMT Attempt regular synthesis with PVA-Alg-NaMT & AC to attempt to integrate AC into the nanocomposite structure Procedure Procedure adapted from | Kuo-Ying Amanda Wu and Keith D. Wisecarver (1992)<br.> <br.> Upscaled PVA-Alg-NaMT<br.> Prepare an aqueous solution of 13% PVA and 0.02% sodium alginate at 60°C (Stir plate on 3rd setting: ~68°C) 4 g of PVA and 0.64 g of sodium alginate in 7 mL of water (12.5% PVA and ~0.02% alginate) Add alginate while stirring PVA-water solution ~0.4 g NaMT should be added to this mixture where applicable Cool dissolved and mixed solution to 35°C Prepare 840 mL of saturated citric acid with 4% calcium chloride Add 33.6 g (4%) calcium chloride to 210 mL of water Add citric acid to saturation (48 g citric acid) 14.7g/100mL > 30.87 g/210 for solubility comparable to boric acid Add the PVA-Alg-Nanocomposite mixture drop-wise (by syringe) to the gently stirring (stir plate 3) citric acid-calcium chloride solution using a Pasteur pipette Stir for 2 hrs to allow solidification Rinse with water to remove excess reactants <br.> PVA-Alg-NaMT&AC Prepare an aqueous solution of 13% PVA and 0.02% sodium alginate at 60°C (Stir plate on 3rd setting: ~68°C) 1 g of PVA and 0.16 g of sodium alginate in 7 mL of water (12.5% PVA and ~0.02% alginate) Add alginate while stirring PVA-water solution ~0.1 g of NaMT and ~0.05 g AC should be added to this mixture where applicable Cool dissolved and mixed solution to 35°C Prepare 210 mL of saturated citric acid with 4% calcium chloride Add 8.4 g (4%) calcium chloride to 210 mL of water Add citric acid to saturation (12-15 g citric acid) 14.7g/100mL > 30.87 g/210 for solubility comparable to boric acid Add the PVA-Alg-Nanocomposite mixture drop-wise (by syringe) to the gently stirring (stir plate 3) citric acid-calcium chloride solution using a Pasteur pipette Stir for 2 hrs to allow solidification Rinse with water to remove excess reactants Measurements PVA-Alg-NaMT PVA: 4.01 g Alg: 0.65 g NaMT: 0.4 g Citric acid: 48.03 g CaCl2: 33.6 g PVA-Alg-NaMT&AC PVA: 1.01 g Alg: 0.16 g NaMT: 0.1 g AC: 0.05 g Citric acid: 12.69 g CaCl2: 8.34 g Notes Run normal-scale PVA-Alg-NaMT with no citric acid Mass out upscaled product, solvent washing and FTIR, pXRD