PNNL

Abstract

A triple containment magic-angle spinning rotor insert system has been developed and a sample handling procedure formulated for safety analyzing highly radioactive solids by high resolution solid state NMR. The protocol and containment system have been demonstrated for magic angle spinning (MAS) experiments on ceramic samples containing 5-10 wt% 239Pu and 238Pu at rotation speeds of 3500 Hz. The technique has been used to demonstrate that MASNMR experiments can be used to measure amorphous atomic number fractions produced during accelerated internal radioactive decay. This will allow incorporated ?-emitters with short half-lives to be used to model the long-term radiation tolerance of potential ceramic radioactive waste forms. It is believed to be the first example of MASNMR spectroscopy on samples containing fissionable isotopes.