A concept to integrate a commercial high-resolution, magic angle spinning nuclear magnetic resonance (MAS-NMR) probe capable of very rapid rotation rates (70 kHz) in a hermetically sealed enclosure for the study of highly radiotoxic materials has been developed and successfully demonstrated. The concept centres on a conventional wide bore (89 mm) solid-state NMR magnet operating with industry standard 54 mm diameter probes designed for narrow bore magnets. Rotor insertion and probe tuning take place within a hermetically enclosed glovebox, which extends into the bore of the magnet, in the space between the probe and the magnet shim system. Oxygen-17 MAS-NMR measurements demonstrate the possibility of obtaining high quality spectra from small sample masses (∼10 mg) of highly radiotoxic material and the need for high spinning speeds to improve the spectral resolution when working with actinides. The large paramagnetic susceptibility arising from actinide paramagnetism in (Th 1−x U x )O 2 solid solutions gives rise to extensive spinning sidebands and poor resolution at 15 kHz, which is dramatically improved at 55 kHz. The first 17 O MAS-NMR measurements on NpO 2+x samples spinning at 55 kHz are also reported. The glovebox approach developed here for radiotoxic materials can be easily adapted to work with other hazardous or even air sensitive materials.

Spark plasma sintering (SPS) is a rapidly developing method for densification of powders into compacts. It belongs to the so-called “field assisted sintering techniques” that enable rapid sintering at much lower temperatures than the classical approaches of pressureless sintering of green pellets or hot isostatic pressing. In this paper, we report the successful integration of a SPS device into a hermetic glovebox for the handling of highly radioactive material containing radioisotopes of U, Th, Pu, Np, and Am. The glovebox implantation has been facilitated by the replacement of the hydraulic system to apply pressure with a compact electromechanical unit. The facility has been successfully tested using UO2 powder. Pellets with 97% of the theoretical density were obtained at 1000 °C for 5 min, significantly lower than the ∼1600 °C for 5-10 h used in conventional pellet sintering.