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In-Depth Compositional Profile Analysis of Alloys Using Optical Emission Glow Discharge Spectrography

Sequential analysis of metal alloys in depths of 0.1 to 40 µm are made with a glow discharge source for optical emission spectrography. The alloys examined have compositional variations in depth due to mass transfer in liquid sodium tests for materials studied in the fast breeder reactor program. The ion-sputtering action of the source produces progressive and discrete sampling of a defined area with concurrent excitation of the analytes in the negative glow region of the discharge. Integrated exposures of successive layers of attack are spectrographically recorded. The total weight loss is measured gravimetrically. Weight loss is assigned per exposure layer, and the depth of each attack is calculated. With more than 98% of the elemental composition measured, the sum of all elements is used as the internal standard. The precision approaches that of the photographic measurement process and does not indicate the ultimate precision of the source.