A new integrated in glove box glow discharge optical emission spectrometer-Application to carbon, nitrogen and oxygen bulk determinations in low alloy steels as a preliminary study

Abstract

A new set-up of a radiofrequency glow discharge spectrometer has been specially designed for glove box adaptation in order to determine light elements in solid nuclear materials such as uranium metal, plutonium metal, mixed uranium and plutonium oxides (MOX) or nuclear waste glasses. Confinement of this type of material must be ensured by a glove box in order to protect the operator from radioactivity (alpha and beta protection) and to prevent contamination of the working area. In this paper, the glow discharge source and the whole system are described; in addition, the operating conditions for low alloy steels, as a preliminary study, are discussed with particular emphasis on sputtering rates and crater profiles. Practical considerations and optimizations are presented in order to improve emission intensities and reproducibility. Calibration graphs were obtained for carbon, nitrogen and oxygen in low alloy steels; detection limits were determined to be 10 µg g ^–1 for carbon, 40 µg g ^–1 for nitrogen and 20 µg g ^–1 for oxygen. Future work that will be necessary before starting bulk and depth-resolved test analyses on conductive and non-conductive nuclear samples is outlined.