Solids-NMR Apparatus for Materials Characterization
Final rept. 15 Sep 96-14 Sep 97
MISSOURI UNIV-KANSAS CITY DEPT OF CHEMISTRY
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Acquire solids nuclear magnetic resonance solids-NMR capability to enable characterization of polymers and other solid state materials of relevance to DoD. Instrumentation Acquired A solids-NMR accessory was acquired for an existing Bruker AC 250 1H resonance at 250 MHz liquids-NMR spectrometer. The acquired equipment included a 35 W buffer amplifier, b 120 W radio frequency RF amplifier for 1H decoupling, c 300 W broadband rf amplifier for non-1H nuclei, and d 7 mm sample diameter 0.300 ml sample volume cross polarization magic angle spinning CP MAS probe with pneumatic control unit. The apparatus was installed and tested by specialists from Bruker Instruments, Billerica, MA. Research Supported by Instrumentation The first solid sample investigated using the newly acquired apparatus was the monomer 1,5,7,11 tetraoxospiro 5,5 undecane, commonly called spiroorthocarbonate0,0. This is an example of a monomer that polymerize without reduction in volume. Research to be Supported by Instrumentation Solids-NMR will be used to help determine the structures of organic polymers and inorganic solid state materials of relevance to DoD. The polymers include ladder- and semi ladder shaped highly conjugated polymers and their monomers, and polyurethane coating materials. The inorganic solids include catalytic zeolites and ferrierites. Relevant nuclei are 27 Al 65 MHz, 13C 63 MHz, 29Si 50 MHz and 15N 25 MHz.
- Test Facilities, Equipment and Methods