User:Karlena L. Brown/Notebook/PVOH Research/2012/09/28

PVOH Research

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OBJECTIVES Run X-ray Diffraction of 50% CEC NaMT, 100% CEC NaMT, and 2:1 Clay-α-Fe3O4 Calculate the amount of Na+ ions in the 2000ppm SO42- solution Calculate the amount of Cu2+ ions in the 2000ppm SO42- solution Calculate the amount of Na+ ions in the 20ppm SO42- solution Calculate the amount of Cu2+ ions in the 20ppm SO42- solution Prepare PVOH 22K films for Glutaldehyde Crosslinking X-Ray Diffraction Instructions Sample Preparation Clean off the low signal background sample holder with a Kimwipe and acetone Using a spatula, scoop and place small amount of finely ground clay sample into sample holder compartment Using a spatula, level off the clay surface in the compartment making an even smooth level plane Wipe the outsides of the compartment of the low signal background sample holder with Kimwipe and acetone again Instrument Programming and Operation Turn on chiller machine Power up X-Ray Diffractometer Set geiger counter 0.1 as a value Check radiation output Open X-Ray Diffractometer instrument door and set sample in sample counter Record sample compartment number in the machine and close the X-ray door Turn on computer, find instrument password, and open STANDARD MEASUREMENT PROGRAM Use the command window to click machine on to connect to the computer Change the file name under Data window to create new folder → CHEM 581 → MKM Create name for sample run under new folder MKM → NaMT Finally save all information and let the sample run begin and continue for 30 minutes X-Ray Diffraction will be run on the following clays: 50% CEC NaMT, 100% CEC NaMT, and the 2:1 α-Fe3O4 X-Ray Diffraction Notes Particle sizes of clay must always be small and finely ground Peaks in clay appear at very low deflection angles (2.5°) NEVER turn off the X-ray coolant in the chiller machine: DAMAGES X-RAY TOOL!!! NEVER rotate powders because sample can fall out!!! All sample run should be run from angles (2 - 40°) at a scanning speed no greater than 1.0 Na+ and Cu2+ Ion Calculations in 2000ppm SO42- Solutions Calculations MW Na2SO4: 142.04 g/mol MW Na+: 22.99 g/mol Mass Na+: 0.00150 g Na2SO4 × (1 mol Na2SO4/142.04 g Na2SO4) × (2 mol Na+/1 mol Na2SO4) × (22.99 g Na+/1 mol Na+) = 4.856 × 10-4 g Na+ Actual concentration of Na+ in 2020 ppm SO4-2 solution: (4.856 × 10-4 g Na+)/0.5 L × 106 = 971 ppm MW CuSO4·5H2O: 249.69 g/mol MW Cu+2: 63.55 g/mol 0.00252 g CuSO4·5H2O × (1 mol CuSO4·5H2O/249.68 g CuSO4·5H2O) × (1 mol Cu+2/1 mol CuSO4·5H2O) × (63.55 g Cu+2/1 mol CuSO4·5H2O) = 6.41 × 10-4 g Cu+2 Actual concentration of Cu+2 in 2020 ppm SO4-2 solution: (6.41 × 10-4 g Cu+2)/0.5 L × 106 = 1283 ppm Cu+2 Na+ and Cu2+ Ion Calculations in 20ppm SO42- Solutions Actual concentration of Na+ in 20 ppm SO4-2 solution: Actual concentration of Na+ in 2020 ppm SO4-2 solution: (4.856 × 10-4 g Na+)/0.5 L × 106 = 971 ppm (971 ppm)(0.00495 L) = (M2)(0.5 L) M2 = 9.61 ppm Na+ Actual concentration of Cu+2 in 20 ppm SO4-2 solution: Actual concentration of Cu+2 in 2020 ppm SO4-2 solution: (6.41 × 10-4 g Cu+2)/0.5 L × 106 = 1283 ppm Cu+2 (1283 ppm)(5.16 mL) = (M2)(0.5 L) M2 = 13.2 ppm Cu+2 Glutaldehyde Films Preparations PROCEDURAL STEPS FOR GLUTALDEHYDE FILM PREPARATION CAN BE FOUND UNDER 9/25/12 Prepared PVOH 22K Films For Crosslinking ' PVOH 22K w/ GA PVOH 22K w/ GA & PDMS PVOH 22K w/ GA & NaMT PVOH 22K w/ GA & 100% CEC NaMT PVOH 22K w/ GA & 50% CEC NaMT Original Mass PVOH used (g) 0.5141 0.9499 0.4880 0.7665 0.4691 Amount of [GA] added (mL) 0.5 0.5 1 1 1 Amount of PDMS added (mL) 0 0.052 0 0 0 Amount of Clay added (g) 0 0 0.1040 0.1022 0.1007